CN111349817A - Titanium alloy drill rod, preparation method and application thereof - Google Patents
Titanium alloy drill rod, preparation method and application thereof Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 191
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 27
- 239000010936 titanium Substances 0.000 claims abstract description 24
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 22
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 62
- 238000005553 drilling Methods 0.000 claims description 26
- 238000000137 annealing Methods 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 229910052721 tungsten Inorganic materials 0.000 claims description 16
- 238000005498 polishing Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 14
- 238000003466 welding Methods 0.000 claims description 13
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 238000005097 cold rolling Methods 0.000 claims description 10
- 238000005242 forging Methods 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 7
- 238000003754 machining Methods 0.000 claims description 7
- 230000008719 thickening Effects 0.000 claims description 7
- 238000001192 hot extrusion Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000011161 development Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 abstract description 36
- 238000005260 corrosion Methods 0.000 abstract description 36
- 230000000052 comparative effect Effects 0.000 description 24
- 239000000203 mixture Substances 0.000 description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 14
- 229910000831 Steel Inorganic materials 0.000 description 12
- 239000010959 steel Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 8
- 239000003345 natural gas Substances 0.000 description 7
- 239000003209 petroleum derivative Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000005096 rolling process Methods 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B17/00—Drilling rods or pipes; Flexible drill strings; Kellies; Drill collars; Sucker rods; Cables; Casings; Tubings
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Physics & Mathematics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to a titanium alloy drill rod, a preparation method and application thereof, wherein the titanium alloy drill rod comprises the following components in percentage by mass: 3-5% of Al; v6-9%; 2 to 7 percent of Cr; 1.5 to 3.5 percent of Mo; 2.5 to 5 percent of Zr; 1-5% of W; 1-5% of Fe; 1 to 5 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti. The titanium alloy drill rod has good high-temperature corrosion resistance and can resist H at the temperature of 150-260 DEG C2S、CO2The annual corrosion rate is reduced to below 0.0006mm/a, and the density is reduced to 4.4-5.8g/cm3The radius of curvature of the whipstock is also reduced to 10-18 meters.
Description
Technical Field
The invention relates to the technical field of petroleum and natural gas drill rods, in particular to a titanium alloy drill rod, a preparation method and application thereof.
Background
With the development of the petroleum and natural gas industry, wells with special working conditions such as deep wells, ultra-deep wells, high-temperature and high-pressure wells, large-displacement horizontal wells, ultra-short curvature radius wells and the like are developed more and more, and the requirements on drilling tools are higher and higher. The drilling is an important link of petroleum and natural gas exploration and development, and the main method adopted at present is a rotary drilling method, wherein a rotary drilling tool is used for transmitting torque to drive a drill bit to rotate, break and cut rocks, the rocks are drilled into the underground, a borehole with a designed depth is drilled, and petroleum or natural gas is obtained. The drill rod is used for transmitting the torque of the drilling machine to the drill bit to realize drilling, is responsible for transmitting drilling fluid and is lifted, lowered and rotated together with the drill bit.
At present, the methodThe steel drill pipe is still the common drill pipe at home and abroad. According to the American Petroleum Institute (API) standard, the steel grades of the steel drill pipe are divided into five grades: D. e, 95(X), 105(G), 135 (S). The higher the steel grade of the steel drill rod, the higher the yield strength of the steel drill rod, and the higher the other strength of the steel drill rod. However, steel drill pipes tend to present a number of problems. First, steel drill rods are not corrosion resistant and are easily exposed to CO2、H2S and other gases are corroded, and the problems of drill pipe breakage, even petroleum and natural gas leakage and the like can be caused after long-term use; secondly, the steel drill rod has higher density, and when the ultra-deep well is exploited, a drilling machine is usually required to be modified to bear the increased quality of the drill rod, so that the exploitation process of petroleum and natural gas is seriously influenced; in addition, the steel drill rod has a large curvature radius, and is often difficult to process ultra-short radius drilling wells or inclined wells.
With the continuous development of titanium alloy, the titanium alloy has the advantages of high strength, small density, high temperature resistance, corrosion resistance, small curvature radius, no magnetism or small magnetism and the like. In response to increasingly complex drilling conditions, titanium alloy drill rods have been developed in the prior art to replace steel drill rods. For example, CN107350618A discloses a friction welding method for a high-strength and high-toughness titanium alloy drill rod material, wherein the titanium alloy drill rod comprises, by weight, 5-7% of Al, 2.0-3.0% of Nb, 0.5-2.0% of Zr, 0.7-1.2% of Mo, 0.02-0.05% of Fe0.01-0.03% of Si, and the balance Ti, but the titanium alloy drill rod has general corrosion resistance and large density and deflection curvature radius, and cannot meet increasingly complex drilling conditions.
CN107747003A discloses a high-strength titanium alloy drill rod and a preparation method thereof, wherein the high-strength titanium alloy drill rod comprises the following components in percentage by mass: 5.5 to 6.8 percent of Al, 3.5 to 4.5 percent of V, less than or equal to 0.3 percent of Fe, less than or equal to 0.15 percent of Si, less than or equal to 0.1 percent of C, less than or equal to 0.05 percent of N, less than or equal to 0.0125 percent of H, less than or equal to 0.2 percent of O, and the balance of Ti, wherein the finished drill rod is obtained after the processes of pressing by a consumable electrode, consumable arc remelting by a vacuum head, secondary remelting, forging and cogging of alloy and rolling of finished bars. Although the titanium alloy drill rod has the advantages of high strength and wear resistance, the titanium alloy drill rod has general corrosion resistance, and both the density and the deflecting curvature radius are large, so that the titanium alloy drill rod cannot meet increasingly complex drilling working conditions.
In summary, there is a need to develop a titanium alloy drill rod with stronger corrosion resistance, smaller density and smaller deflecting curvature radius and a preparation method thereof so as to meet increasingly complex drilling conditions.
Disclosure of Invention
In order to solve the technical problems, the invention provides the titanium alloy drill rod, which improves the high-temperature corrosion resistance and reduces the density and the deflecting curvature radius on the basis of meeting the performance standards of yield strength, tensile strength, elongation, impact power of a V-shaped Charpy longitudinal full-size sample and the like by optimizing the composition proportion of the titanium alloy, is suitable for various complex drilling working conditions, fills in domestic blank, and has wide application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a titanium alloy drill rod, which comprises the following components in percentage by mass: 3-5% of Al; v6-9%; 2 to 7 percent of Cr; 1.5 to 3.5 percent of Mo; 2.5 to 5 percent of Zr; 1-5% of W; fe 1-5%; 1 to 5 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
According to the invention, through the coordination effect among the components of Al, V, Cr, Mo, Zr, W, Fe, Si and Ti with specific contents, the performance of the titanium alloy is improved, and particularly on the basis of the specific contents of the five elements of Cr, Mo, Zr, W and Fe, the specific addition proportion among the elements is controlled, so that the prepared titanium alloy drill rod obtains good high-temperature corrosion resistance, lower density and lower deflecting curvature radius, and has good mechanical properties.
According to the invention, based on the excellent performances of five elements of Cr, Mo, Zr, W and Fe, the mass proportion of Fe and Cr and the mass proportion of Mo, Zr and W are further controlled, and then the components are mixed with Al, V, Si and Ti to prepare the titanium alloy, so that a synergistic effect is generated among the components, and further the high-temperature corrosion resistance, the density and the deflecting curvature radius can be greatly optimized.
The C element, the N element, the H element and the O element are inevitable impurities in actual production, and the content of the C element, the N element, the H element and the O element is controlled within the range, so that the performance of the finally prepared titanium alloy drill rod cannot be influenced, and further description is omitted.
The titanium alloy drill rod of the present invention has an Al content of 3 to 5% by mass, for example, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.3%, 4.5%, 4.7%, or 5%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
According to the titanium alloy drill rod, the mass percentage of the Al element is controlled to be 3-5%, so that the high-temperature corrosion resistance of the titanium alloy drill rod is improved, the density and the deflecting curvature radius of the titanium alloy drill rod are reduced, and the titanium alloy drill rod has a wider application range.
The titanium alloy drill rod of the present invention has a V content of 6-9% by mass, for example, 6%, 6.5%, 7%, 7.5%, 8%, 8.5% or 9%, but not limited to the recited values, and other values not recited within the range of values are also applicable.
According to the titanium alloy drill rod, the mass percentage of the V element is controlled to be 6-9%, the high-temperature corrosion resistance and the deflecting curvature radius of the titanium alloy drill rod can be effectively improved while the β phase is subjected to solid solution strengthening, and the titanium alloy drill rod plays a key role in reducing the deflecting curvature radius.
The titanium alloy drill rod according to the present invention has a Cr content of 2 to 7% by mass, for example, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, or 7%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
The titanium alloy drill rod of the present invention has a Fe content of 1 to 5% by mass, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
For the invention, within the mass percentage content range of the Cr element and the Fe element, the mass ratio of the Cr element to the Fe element in the titanium alloy needs to be further controlled within the range of 2-4:1, so that the Cr element and the Fe element generate a synergistic effect mutually and are matched with Mo, Zr and W under a specific mass ratio, and the high-temperature corrosion resistance and the deflecting curvature radius of the titanium alloy drill rod can be greatly optimized.
The mass ratio of the Cr element to the Fe element in the present invention is 2-4:1, for example, 2:1, 2.5:1, 3:1, 3.5:1 or 4:1, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
The content of Mo in the titanium alloy drill rod according to the present invention is 1.5 to 3.5% by mass, for example, 1.5%, 1.7%, 2%, 2.2%, 2.4%, 2.5%, 2.7%, 3%, 3.3%, or 3.5%, etc., but is not limited to the recited values, and other values not recited in the above range are also applicable.
The mass percentage of Zr in the titanium alloy drill rod according to the present invention is 2.5-5%, for example, 2.5%, 2.7%, 3%, 3.3%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 4.6%, 4.8%, or 5%, etc., but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
The titanium alloy drill rod according to the present invention has a W content of 1 to 5% by mass, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
For the present invention, within the mass percentage content range of Mo, Zr and W, the mass ratio of Mo, Zr and W in the titanium alloy needs to be further controlled within the range of (1.5-3.5):1, so that the Mo, Zr and W generate a synergistic effect with each other, and together with the Cr element and the Fe element which also have specific mass ratios, the high temperature corrosion resistance and the deflecting curvature radius of the titanium alloy drill rod can be effectively improved.
The mass ratio of Mo, Zr and W in the present invention is (1.5-3.5):1, for example, 1.5:1.5:1, 2:1.5:1, 2.5:1.7:1, 3:2.5:1 or 3.5:3.5:1, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
The titanium alloy drill rod according to the present invention has a Si content of 1 to 5% by mass, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
In the prior art, Si element is usually set as impurity element, and the content of the impurity element is reduced as much as possible, but the titanium alloy drill rod can effectively stabilize β phase by controlling the mass percentage of the Si element to be 1-5%, thereby enhancing the strength, the high-temperature corrosion resistance and the deflecting curvature radius of the titanium alloy drill rod.
The titanium alloy drill rod disclosed by the invention contains C, N, H, O and other impurity elements besides Al, V, Cr, Mo, Zr, W, Fe and Si, and the balance Ti means that all the components except the eight alloy components and the four impurity components are Ti.
As a preferable technical scheme of the invention, the titanium alloy drill rod comprises the following components in percentage by mass: 3.5 to 4.5 percent of Al; v6-8%; 2.7 to 6 percent of Cr; 2 to 3.5 percent of Mo; 2.5 to 4.5 percent of Zr; 1-4% of W; 2 to 4.5 percent of Fe; 1 to 4.5 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
As a preferable technical scheme of the invention, the titanium alloy drill rod comprises the following components in percentage by mass: 4 to 4.5 percent of Al; v6-7.3%; 3.5 to 5.5 percent of Cr; 2.5 to 3.5 percent of Mo; 2.5 to 3.5 percent of Zr; 1 to 2.5 percent of W; fe 2-3%; 1 to 3 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
The selected preferred component content can improve the mechanical strength of the titanium alloy drill rod, and further improve the high-temperature corrosion resistance, the density and the deflecting curvature radius of the titanium alloy.
In a preferred embodiment of the present invention, the titanium alloy drill rod has a yield strength of 510-.
Preferably, the titanium alloy drill rod has a tensile strength of 600-1300MPa, such as 600MPa, 700MPa, 800MPa, 900MPa, 1000MPa, 1100MPa, 1200MPa, or 1300MPa, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the titanium alloy drill rod has an elongation of 12% or more, such as 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24% or 25%, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the V-shaped Charpy longitudinal full-size test piece of the titanium alloy drill rod has impact energy of more than or equal to 50J, such as 50J, 55J, 60J, 65J, 70J, 75J or 80J, and the like, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the product specification range of the titanium alloy drill rod according to the length of the wall thickness × with the outer diameter × is 60.3-600mm × 5-25mm × 6000-12000mm, and the titanium alloy drill rod can be reasonably selected by a person skilled in the art according to actual conditions.
The second purpose of the invention is to provide a preparation method of the titanium alloy drill rod, which comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) performing polishing, hot piercing or hot extrusion on the titanium alloy bar obtained in the step (1) in sequence to prepare a titanium alloy tube blank, and then performing cold rolling, annealing, hot straightening, upsetting and heat treatment in sequence to obtain a titanium alloy tube body;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) friction welding the titanium alloy pipe body obtained in the step (2) and the titanium alloy joint obtained in the step (3), and then sequentially carrying out inner and outer flash and weld heat treatment to obtain the titanium alloy drill rod;
wherein, the step (2) and the step (3) have no sequence.
In a preferred embodiment of the present invention, the number of cold rolling passes in step (2) is 2 to 7, for example, 2, 3, 4, 5, 6 or 7, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
The cold rolling passes refer to rolling by a rolling mill, and the rolling deformation of one pass is 20-80 percent.
Preferably, the annealing in step (2) includes vacuum annealing and/or oxidation annealing, and the person skilled in the art can make reasonable selection according to the actual situation.
Preferably, the heating temperature of the annealing in step (2) is 600-.
Preferably, the annealing in step (2) is carried out at a holding time of 35-65min, such as 35min, 37min, 40min, 42min, 45min, 48min, 50min, 52min, 55min, 58min, 60min, 62min or 65min, but not limited to the values listed, and other values not listed in the range of values are also applicable.
The heat preservation time of the annealing in the step (2) of the invention is calculated according to the following formula:
and (3) keeping the temperature for 5.6 × (the wall thickness of the titanium alloy pipe body) min + (30-40) min, wherein the unit of the wall thickness of the titanium alloy pipe body is mm.
As a preferred embodiment of the present invention, the heating temperature for the upsetting in the step (2) is 800-.
Preferably, the upsetting mode in the step (2) is inner-outer upsetting or outer-outer upsetting, and a person skilled in the art can reasonably select the upsetting mode according to actual conditions.
The polishing treatment in the step (2) and the step (3) aims to remove the defects such as oxide skin and cracks of the titanium alloy bar obtained after forging by using a lathe.
In a preferred embodiment of the present invention, both the heat treatment in step (2) and the heat treatment in step (3) are performed by any one of the following heat treatment systems:
a) preserving heat for 0.5-3h at 600-;
b) keeping the temperature at 600-;
c) preserving the heat for 0.5-3h at the temperature of 600-;
d) keeping the temperature at 600-1100 ℃ for 0.5-3h, performing air cooling in a first-out furnace, then returning the furnace and keeping the temperature at 450-750 ℃ for 2-6h, and performing air cooling after the furnace is taken out again.
In the invention, the four heat treatment systems of a), b), c) and d) are kept at the temperature of 600-1100 ℃ for 0.5-3h, wherein the temperature is 600-1100 ℃, such as 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ or 1100 ℃, and the like, and the keeping time is 0.5-3h, such as 0.5h, 1h, 1.5h, 2h, 2.5h or 3h, and the like, but the above range is not limited to the enumerated values, and other unrecited values in the range are also applicable.
The furnace temperature in the heat treatment system c) of the present invention is as low as 300 ℃ and 800 ℃, for example, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃ or 800 ℃, but the present invention is not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
The annealing temperature in the heat treatment system d) of the present invention is 450-750 ℃, for example, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ or 750 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
The annealing holding time in the heat treatment system d) of the present invention is 2 to 6 hours, for example, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours or 6 hours, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
The four heat treatment systems of a), b), c) and d) are designed according to the composition content of the titanium alloy, so that the titanium alloy pipe body and the titanium alloy joint can be effectively ensured to meet the requirement on mechanical strength in the preparation process, and further the yield strength, the tensile strength, the elongation and the impact function of the V-shaped Charpy longitudinal full-size sample of the titanium alloy drill rod can meet the quality requirement.
As a preferable technical scheme of the invention, the friction welding in the step (4) adopts a mode that the titanium alloy pipe body is fixed and the titanium alloy joint rotates.
Preferably, the rotation speed of the titanium alloy joint is 325-1000r/min, such as 325r/min, 350r/min, 400r/min, 450r/min, 500r/min, 600r/min, 700r/min, 800r/min, 850r/min, 900r/min, 950r/min or 1000r/min, but not limited to the enumerated values, and other unrecited values within the numerical range are also applicable.
Preferably, the heating temperature of the heat treatment of the welding seam in the step (4) is 820-.
Preferably, the holding time of the heat treatment of the welding seam in the step (4) is 10-18min, such as 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min or 18min, but not limited to the enumerated values, and other unrecited values in the range of the enumerated values are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) polishing, hot piercing or hot extrusion are sequentially carried out on the titanium alloy bar obtained in the step (1) to prepare a titanium alloy tube blank, then a cold rolling pass is carried out for 2-7 times, then the heat preservation is carried out for 35-65min at 950 ℃ in a vacuum annealing and/or oxidation annealing mode, then the upsetting treatment is carried out on the titanium alloy tube blank after the thermal straightening treatment at 1250 ℃ in a mode of internal and external thickening or external thickening, and finally the titanium alloy tube body is obtained through the heat treatment;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) fixing the titanium alloy pipe body obtained in the step (2), performing friction welding on the titanium alloy joint obtained in the step (3) by rotating, controlling the rotating speed to be 325-;
wherein, the step (2) and the step (3) have no sequence.
In the preparation method of the titanium alloy drill rod, various equipment and technical means are common equipment and conventional methods in the field, and the preparation method is not limited too much.
The invention also aims to provide application of the titanium alloy drill pipe, which is used for exploration and development of petroleum and natural gas drilling and is suitable for various complex drilling working conditions.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the titanium alloy drill rod has good high-temperature corrosion resistance and can resist H at the temperature of 150-260 DEG C2S、CO2The annual corrosion rate is reduced to below 0.0006 mm/a;
(2) the titanium alloy drill rod has low density which is only 4.4-5.8g/cm3When the ultra-deep well is exploited, a drilling machine does not need to be modified, and the number of drill rods is directly increased;
(3) the deflecting curvature radius of the titanium alloy drill rod is 10-18m, and the titanium alloy drill rod is suitable for ultra-short radius drilling or inclined wells;
(4) the titanium alloy drill rod also meets the performance standards of yield strength of 510-1040MPa, tensile strength of 600-1300MPa, elongation of more than or equal to 12%, impact energy of a V-shaped Charpy longitudinal full-size sample of more than or equal to 50J and the like, fills the domestic blank, and has wide application prospect.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a titanium alloy drill rod which comprises the following components in percentage by mass: al 4%; v6%; 5% of Cr; mo is 3 percent; 2.5 percent of Zr; 1.5 percent of W; fe2 percent; 1% of Si; 0.08 percent of C; 0.04 percent of N; 0.01 percent of H; 0.2 percent of O; the balance being Ti.
The preparation method of the titanium alloy drill rod comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) performing polishing, hot piercing or hot extrusion on the titanium alloy bar obtained in the step (1) in sequence to prepare a titanium alloy tube blank, then performing cold rolling pass for 5 times, then performing heat preservation for 50min at 750 ℃ in a vacuum annealing mode, then performing upsetting treatment on the titanium alloy tube blank subjected to the heat straightening treatment at 1000 ℃ in an internal and external thickening mode, and finally performing heat treatment to obtain a titanium alloy tube body;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) fixing the titanium alloy pipe body obtained in the step (2), performing friction welding by rotating the titanium alloy joint obtained in the step (3), controlling the rotating speed to be 800r/min, and after finishing the inner and outer flash treatment, performing heat preservation at 850 ℃ for 15min to perform weld heat treatment to obtain the titanium alloy drill rod;
wherein, the heat treatment in the step (2) and the heat treatment in the step (3) both adopt a) heat treatment system, namely heat preservation is carried out for 2 hours at 1000 ℃, then furnace cooling is carried out to below 100 ℃, and air cooling is carried out after discharge;
wherein, the step (2) and the step (3) have no sequence.
Example 2
The embodiment provides a titanium alloy drill rod which comprises the following components in percentage by mass: 3.5 percent of All; v8%; 6 percent of Cr; 3.5 percent of Mo; 2.5 percent of Zr; w1%; fe 3 percent; 4.5 percent of Si; 0.1 percent of C; 0.04 percent of N; 0.015 percent of H; 0.2 percent of O; the balance being Ti.
The preparation method of the titanium alloy drill rod comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) performing polishing, hot piercing or hot extrusion on the titanium alloy bar obtained in the step (1) in sequence to prepare a titanium alloy tube blank, then performing cold rolling pass for 2 times, then performing heat preservation for 35min at 600 ℃ in an oxidation annealing mode, then performing upsetting treatment on the titanium alloy tube blank subjected to the thermal straightening treatment at 800 ℃ in an external thickening mode, and finally performing heat treatment to obtain a titanium alloy tube body;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) fixing the titanium alloy pipe body obtained in the step (2), performing friction welding by rotating the titanium alloy joint obtained in the step (3), controlling the rotating speed to be 325r/min, and after finishing the inner and outer flash treatment, performing heat preservation at 820 ℃ for 10min to perform weld heat treatment to obtain the titanium alloy drill rod;
wherein, the heat treatment in the step (2) adopts a b) heat treatment system, namely, the heat is preserved for 3 hours at the temperature of 600 ℃, and the mixture is directly discharged from the furnace for air cooling; the heat treatment in the step (3) adopts a c) heat treatment system, namely heat preservation is carried out for 2.5 hours at 700 ℃, then furnace cooling is carried out to 300 ℃, and air cooling is carried out after discharging;
wherein, the step (2) and the step (3) have no sequence.
Example 3
The embodiment provides a titanium alloy drill rod which comprises the following components in percentage by mass: al 5%; v9%; cr 7 percent; 3.5 percent of Mo; 3.5 percent of Zr; w1%; fe2 percent; 1% of Si; 0.05 percent of C; 0.05 percent of N; h0.012%; 0.25 percent of O; the balance being Ti.
The preparation method of the titanium alloy drill rod comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) polishing, hot piercing or hot extruding the titanium alloy bar obtained in the step (1) in sequence to prepare a titanium alloy tube blank, then carrying out cold rolling pass for 7 times, then carrying out heat preservation for 65min at 950 ℃ in an oxidation annealing mode, then carrying out upsetting treatment on the titanium alloy tube blank subjected to the thermal straightening treatment at 1250 ℃ in an external thickening mode, and finally carrying out heat treatment to obtain a titanium alloy tube body;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) fixing the titanium alloy pipe body obtained in the step (2), performing friction welding by rotating the titanium alloy joint obtained in the step (3), controlling the rotating speed to be 1000r/min, and after finishing the inner and outer flash treatment, performing heat preservation at 940 ℃ for 18min to perform weld heat treatment to obtain the titanium alloy drill rod;
wherein, the heat treatment in the step (2) and the heat treatment in the step (3) both adopt a d) heat treatment system, namely heat preservation is carried out for 0.5h at 1100 ℃, air cooling is carried out in a first furnace, then heat preservation is carried out for 4h at 500 ℃ in a second furnace, and air cooling is carried out after the furnace is taken out again;
wherein, the step (2) and the step (3) have no sequence.
Example 4
The conditions were exactly the same as in example 1 except that the composition was changed to "Cr 5%, Fe 2%" and "Cr 5%, Fe 3%" (the mass ratio of Cr to Fe was 1.67:1) and the Ti content was reduced adaptively and equally in comparison with example 1.
Example 5
The conditions were exactly the same as in example 1 except that the composition was changed to "Cr 5%, Fe 2%" and "Cr 5%, Fe 1%" (the mass ratio of Cr to Fe was 5:1) and the Ti content was increased adaptively and equally in comparison with example 1.
Example 6
The conditions were exactly the same as in example 1 except that "Mo 3%, Zr 2.5%, W1.5%" was changed to "Mo2.5%, Zr 2.5%, W2%" (the mass ratio of Mo, Zr and W was 1.25:1.25:1) in the composition of the components, as compared with example 1.
Example 7
The conditions were exactly the same as in example 1 except that "Mo 3%, Zr 2.5%, W1.5%" was changed to "Mo 3.5%, Zr 4%, W1%" (the mass ratio of Mo, Zr, and W was 3.5:4:1) in the composition of the components, and the content of Ti was reduced adaptively and equally.
Comparative example 1
The conditions were exactly the same as in example 1 except that "Al 4%" was changed to "Al 2%" in the composition, and the Ti content was increased adaptively and equally in the composition in comparison with example 1.
Comparative example 2
The conditions were exactly the same as in example 1 except that "Al 4%" was changed to "Al 6%" in the composition, and the Ti content was reduced adaptively and equally in comparison with example 1.
Comparative example 3
The conditions were exactly the same as in example 1 except that "V6%" was changed to "V5%" in the composition of the components, and the content of Ti was increased adaptively and equally.
Comparative example 4
The conditions were exactly the same as in example 1 except that "V6%" was changed to "V10%" in the composition of the components and the content of Ti was reduced adaptively and equally as in example 1.
Comparative example 5
The conditions were exactly the same as in example 1 except that "Si 1%" was changed to "Si 0.05%" in the composition of the composition, and the content of Ti was increased adaptively and equally in comparison with example 1.
Comparative example 6
The composition of the titanium alloy drill rod of this comparative example was the same as that of example 1.
The preparation method of the titanium alloy drill rod comprises the following steps:
compared with the example 1, the conditions are completely the same as the example 1 except that the heat treatment system of a) keeping the temperature at 1000 ℃ for 2h, then cooling the furnace to below 100 ℃ and taking out the furnace and then performing air cooling is adopted for the heat treatment of the step (2) and the heat treatment of the step (3), and the heat treatment system of keeping the temperature at 500 ℃ for 2h, cooling the furnace to below 100 ℃ and taking out the furnace and performing air cooling is replaced by the following heat treatment system.
Comparative example 7
The composition of the titanium alloy drill rod of this comparative example was the same as that of example 1.
The preparation method of the titanium alloy drill rod comprises the following steps:
compared with the example 1, the conditions are completely the same as the example 1 except that the heat treatment system of a) keeping the temperature at 1000 ℃ for 2h, then cooling the furnace to below 100 ℃ and taking out the furnace and then performing air cooling is adopted for the heat treatment of the step (2) and the heat treatment of the step (3), and the heat treatment system of keeping the temperature at 1200 ℃ for 2h, cooling the furnace to below 100 ℃ and taking out the furnace and performing air cooling is replaced by the following heat treatment system.
The titanium alloy drill rods obtained in the above examples and comparative examples were subjected to the following performance tests:
and (3) corrosion resistance testing: placing the prepared titanium alloy drill rod sample in H2S、CO2The corrosion weight loss is tested in the temperature range of 150-260 ℃ under partial pressure. The test evaluation standard calculates the annual corrosion rate according to the mass difference of the sample before and after corrosion, and the corrosion degree of the sample is judged according to NACE standard RP-0775-91;
and (3) testing the density: weighing the prepared titanium alloy drill rod sample to obtain the mass m of the sample; then putting the sample into a measuring cylinder filled with a certain volume of water, and obtaining the volume V of the sample through volume increment; finally, calculating the density rho of the titanium alloy drill rod sample according to a density formula rho-m/V;
and (3) testing the deflecting curvature radius: for the surface, the curvature radius is the radius of a circle which is most suitable for a normal section or a combination thereof, so that the length of a curved surface and an unbent end surface of a titanium alloy drill rod sample is measured by adopting a length ruler to obtain the corresponding deflecting curvature radius;
and (3) testing mechanical properties:
the yield strength, the tensile strength and the elongation of a titanium alloy drill rod sample and the impact power of a V-shaped Charpy longitudinal full-size sample are tested, and the test standard is as follows: ASTM E8/E8M-11; GB/T228.1: 2010; JIS Z2241-2011;
the experimental conditions are as follows:
total test pressure: 25 MPa; temperature: 150 ℃ and 260 ℃; h2S partial pressure: 7 MPa; CO 22Partial pressure: 11MPa test time: 720 hours.
The titanium alloy drill pipe samples prepared in examples 1-7 and comparative examples 1-7 are tested by the corrosion resistance testing method, wherein the experiment temperature is set to be 200 ℃ in example 2, 150 ℃ in example 3 and 260 ℃ in other examples and comparative examples, the samples are weighed before and after corrosion, and the annual corrosion rate is calculated; the density, the deflecting curvature radius, the yield strength, the tensile strength, the elongation and the impact energy of the V-shaped Charpy longitudinal full-size test sample are tested at room temperature, and the test results are shown in Table 1.
TABLE 1
From table 1, the following points can be obtained:
(1) examples 1-7 titanium alloy drill rods prepared according to the formulation described herein have good high temperature corrosion resistance to H at 150-260 deg.C2S、CO2The annual corrosion rate is reduced to below 0.0006mm/a, and the density is reduced to 4.4-5.8g/cm3The deviation-making curvature radius is reduced to 10-18m, so that the method is suitable for various complex drilling working conditions, fills the domestic blank and has wide application prospect; in addition, the performance standards of 510-1040MPa yield strength, 600-1300MPa tensile strength and 12% elongation are met, wherein the impact energy of the V-shaped Charpy longitudinal full-size test sample is more than or equal to 50J and is better than that of the prior art, namely 47Performance criteria for J;
(2) comparing example 1 with examples 4 and 5, it can be seen that: in the embodiment 1, the mass ratio of Cr element to Fe element in the titanium alloy drill rod is controlled within the range of 2-4:1, and the optimization is realized on the high-temperature corrosion resistance, the density and the deflecting curvature radius;
(3) comparing example 1 with examples 6 and 7, it can be seen that: in the embodiment 1, the mass ratio of Mo, Zr and W in the titanium alloy drill rod is controlled within the range of (1.5-3.5):1, the high-temperature corrosion resistance, the density and the deflecting curvature radius are optimized, and particularly, the density and the deflecting curvature radius are greatly reduced;
(4) comparing example 1 with comparative examples 1, 2, it can be seen that: the comparative example 1 reduces the content of Al element to 2%, and the obtained titanium alloy drill rod has poor corrosion resistance and deflecting curvature radius, and also causes the reduction of strength and impact toughness; the comparative example 2 increases the content of Al element to 6%, and the obtained titanium alloy drill rod has the defects of poor corrosion resistance and deflecting curvature radius and poor hot workability;
(5) comparing example 1 with comparative examples 3, 4, it can be seen that: comparative example 3 the content of the element V is reduced to 5%, the obtained titanium alloy drill rod not only has poor corrosion resistance and deflecting curvature radius, but also causes the reduction of strength and ductility; comparative example 4 increasing the content of V element to 10%, the obtained titanium alloy drill rod was not only inferior in corrosion resistance, density and deflecting curvature radius, but also decreased in shrinkage property although the strength was increased;
(6) comparing the example 1 with the comparative example 5, it can be seen that, similar to the prior art, the comparative example 5 reduces the content of the Si element to the content level of the impurity element, and cannot play a role in stabilizing the β phase, so that the corrosion resistance, the density, the deflecting curvature radius and the strength of the obtained titanium alloy drill rod are poor, wherein both the elongation and the impact power cannot reach the performance standards;
(7) comparing example 1 with comparative examples 6, 7, it can be seen that: the heat treatment system of the comparative example 6 adopts a lower temperature, and does not reach a state of complete recrystallization of crystal grains, so that the mechanical property of the titanium alloy drill rod can not reach the performance standard; the heat treatment system of the comparative example 7 adopts higher temperature, so that the crystal grains grow abnormally, the titanium alloy drill rod is easy to break when in use, and huge potential safety hazards exist; in addition, the titanium alloy drill rods obtained in comparative examples 6 and 7 were inferior in corrosion resistance, density, and deflecting radius of curvature.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The titanium alloy drill rod is characterized by comprising the following components in percentage by mass: 3-5% of Al; v6-9%; 2 to 7 percent of Cr; 1.5 to 3.5 percent of Mo; 2.5 to 5 percent of Zr; 1-5% of W; 1-5% of Fe; 1 to 5 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
2. The titanium alloy drill rod as claimed in claim 1, wherein the titanium alloy drill rod consists of the following components in percentage by mass: 3.5 to 4.5 percent of Al; v6-8%; 2.7 to 6 percent of Cr; 2 to 3.5 percent of Mo; 2.5 to 4.5 percent of Zr; 1-4% of W; 2 to 4.5 percent of Fe; 1 to 4.5 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
3. The titanium alloy drill rod as claimed in claim 1 or 2, wherein the titanium alloy drill rod consists of the following components in percentage by mass: 4 to 4.5 percent of Al; v6-7.3%; 3.5 to 5.5 percent of Cr; 2.5 to 3.5 percent of Mo; 2.5 to 3.5 percent of Zr; 1 to 2.5 percent of W; 2-3% of Fe; 1 to 3 percent of Si; c is less than or equal to 0.1 percent; n is less than or equal to 0.05 percent; h is less than or equal to 0.015 percent; o is less than or equal to 0.25 percent; the balance being Ti.
4. The titanium alloy drill rod as recited in any one of claims 1 to 3, wherein the yield strength of the titanium alloy drill rod is 510-;
preferably, the tensile strength of the titanium alloy drill rod is 600-1300 MPa;
preferably, the elongation of the titanium alloy drill rod is more than or equal to 12 percent;
preferably, the impact energy of the V-shaped Charpy longitudinal full-size test sample of the titanium alloy drill rod is more than or equal to 50J.
5. A method for manufacturing a titanium alloy drill rod according to any one of claims 1 to 4, characterized in that the method comprises the following steps:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) performing polishing, hot piercing or hot extrusion on the titanium alloy bar obtained in the step (1) in sequence to prepare a titanium alloy tube blank, and then performing cold rolling, annealing, hot straightening, upsetting and heat treatment in sequence to obtain a titanium alloy tube body;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) friction welding the titanium alloy pipe body obtained in the step (2) and the titanium alloy joint obtained in the step (3), and then sequentially carrying out inner and outer flash and weld heat treatment to obtain the titanium alloy drill rod;
wherein, the step (2) and the step (3) have no sequence.
6. The manufacturing method according to claim 5, wherein the cold rolling of step (2) is performed in 2 to 7 passes;
preferably, the annealing of step (2) comprises vacuum annealing and/or oxidation annealing;
preferably, the heating temperature of the annealing in the step (2) is 600-950 ℃;
preferably, the heat preservation time of the annealing in the step (2) is 35-65 min;
preferably, the heating temperature of the upsetting in the step (2) is 800-;
preferably, the upsetting mode of the step (2) is internal and external upsetting or external upsetting.
7. The production method according to claim 5 or 6, wherein the heat treatment in step (2) and the heat treatment in step (3) are performed by any one of the following heat treatment systems:
a) preserving heat for 0.5-3h at 600-;
b) keeping the temperature at 600-;
c) preserving the heat for 0.5-3h at the temperature of 600-;
d) keeping the temperature at 600-1100 ℃ for 0.5-3h, performing air cooling in a first-out furnace, then returning the furnace and keeping the temperature at 450-750 ℃ for 2-6h, and performing air cooling after the furnace is taken out again.
8. The manufacturing method according to any one of claims 5 to 7, wherein the friction welding in the step (4) is performed by fixing the titanium alloy pipe body and rotating the titanium alloy joint;
preferably, the rotation speed of the titanium alloy joint is 325-1000 r/min;
preferably, the heating temperature of the welding seam heat treatment in the step (4) is 820-;
preferably, the heat preservation time of the weld joint heat treatment in the step (4) is 10-18 min.
9. The method according to any one of claims 5 to 8, characterized by comprising the steps of:
(1) batching according to the target mass ratio of the titanium alloy, and then sequentially smelting and forging to obtain a titanium alloy bar;
(2) polishing, hot piercing or hot extrusion are sequentially carried out on the titanium alloy bar obtained in the step (1) to prepare a titanium alloy tube blank, then a cold rolling pass is carried out for 2-7 times, then the heat preservation is carried out for 35-65min at 950 ℃ in a vacuum annealing and/or oxidation annealing mode, then the upsetting treatment is carried out on the titanium alloy tube blank after the thermal straightening treatment at 1250 ℃ in a mode of internal and external thickening or external thickening, and finally the titanium alloy tube body is obtained through the heat treatment;
(3) sequentially carrying out heat treatment, polishing, hole drilling or upsetting on the titanium alloy bar obtained in the step (1) to obtain a drill rod joint blank, and then carrying out thread machining to obtain a titanium alloy joint;
(4) fixing the titanium alloy pipe body obtained in the step (2), performing friction welding on the titanium alloy joint obtained in the step (3) by rotating, controlling the rotating speed to be 325-;
wherein, the step (2) and the step (3) have no sequence.
10. Use of a titanium alloy drill pipe according to any one of claims 1 to 4 in a well for exploration and development of oil and gas.
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Effective date of registration: 20221115 Address after: 617000 Panzhihua vanadium titanium high tech Industrial Development Zone, Sichuan Province Patentee after: ZHONGSHI TITANIUM INDUSTRY CO.,LTD. Patentee after: Zhong Xin hi tech material Limited by Share Ltd. Address before: 617000 Panzhihua vanadium titanium high tech Industrial Development Zone, Sichuan Province Patentee before: ZHONGSHI TITANIUM INDUSTRY CO.,LTD. |