CN104120317A - Magnesium alloy, preparation method and application thereof - Google Patents
Magnesium alloy, preparation method and application thereof Download PDFInfo
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- CN104120317A CN104120317A CN201310146529.XA CN201310146529A CN104120317A CN 104120317 A CN104120317 A CN 104120317A CN 201310146529 A CN201310146529 A CN 201310146529A CN 104120317 A CN104120317 A CN 104120317A
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Abstract
The invention provides a magnesium alloy, and in particular magnesium alloy with a core-shell structure. The magnesium alloy comprises the following components by mass percentage: 5-24% of Al, 0.05-10% of Fe, 0.2-5% of Zn, 0.1-0.7% of Zr, 0-0.2% of Mn and the balance of Mg, wherein the total sum of the components is 100%. The magnesium alloy provided by the invention is especially suitable for application to the pressure ball material in the exploitation of oil and gas. The invention also provides a preparation method of the magnesium alloy. The invention employs reasonable mixture ratio of the components and simple production process, and can effectively improve the overall strength and decomposition properties of the magnesium alloy. The invention uses a high-energy ball milling and vacuum hot pressing sintering methods to obtain a powdered metallurgy magnesium alloy with fine grains, so that the performance of the magnesium alloy can meet the requirements of pressure ball material for petroleum and natural gas exploitation on the strength and decomposition performance; and the invention expands the application of the magnesium alloy in the exploitation of oil and natural gas, and provides powdered metallurgy magnesium alloy, which can be used in industrial application.
Description
Technical field
The present invention relates to a kind of magnesium alloy, its preparation method and application thereof, be specifically related to a kind of decomposable nucleocapsid structure formula magnesium alloy, can be used as the ball material that builds the pressure of oil-gas mining.
Background technology
Shale gas refers to compose and is stored in rich organic mud shale and interlayer thereof, take and adsorbs or unconventional Sweet natural gas that unbound state is main existing way, and composition be take methane as main, is a kind of clean, Energy resources efficiently.In recent years, U.S.'s shale gas exploratory development technological breakthrough, output rapid growth, produces great effect to international market for natural gas and world energy sources general layout, and world Main Resources state has all strengthened the exploratory development dynamics to shale gas.Multistage sliding sleeve staged fracturing technology is the Novel oil gas stimulation technology that Oil-Gas Well Engineering technical field grows up in recent years, is mainly used in orientation well, the fractured horizontal well volume increase transformation of shale gas and low permeability reservoir.This technology can be according to the needs of stratum geological state and reservoir exploitation, adopt pkr that horizontal well is separated into some sections, by ground pitching control device, in well, drop into successively the ascending ball that builds the pressure of diameter, open step by step sliding sleeve, targetedly rock in pay zone is carried out to pressure break, form oil, Sweet natural gas fluid crack passage, to expand layer of oil gas production drainage area, improve the rate of oil and gas recovery.In this technology, one of key part is the sliding sleeve ball that builds the pressure, and its major function is: 1) open sliding sleeve payzone is carried out to pressure break; 2) isolation bottom reservoir.After all payzone pressure breaks finish, utilize the reservoir pressure ball that will build the pressure to return discharge well head, or use drilling tool that sliding sleeve tee and the round bur that builds the pressure are fallen, the weak point of these methods is, be subject to the impact of reservoir pressure and site operation pressure, the ball generation screens that may cause building the pressure, the row of returning is unsuccessful, be lowered to drilling tool and carry out milling meeting prolongation construction period, increase construction cost and risk.Therefore, develop and a kind ofly can bear pressing crack construction high pressure, shaft bottom high temperature, and the ball material that builds the pressure that can decompose voluntarily under in-hole fluid environment, can effectively reduce construction risk, improve operating efficiency.
U.S. Patent Publication a kind of nucleocapsid structure formula composite material and preparation method thereof (United States Patent (USP) of decomposable multilayer coating structure, US2011/0132143A1,2011), this patent shows, by the surface at nano level nucleome metal (as magnesium, aluminium, zinc, manganese and alloy thereof) powder particle, adopt the method for fluidized-bed electroless plating, plate the nano level shell of multilayer different metal or burning, as Al, Ni, Al
2o
3deng, and then composite powder after coating is carried out to sintering, acquisition has the nano composite material of certain decomposability, but the method requires at the higher nano level magnesium of specific activity, aluminium, zinc, manganese and alloy surface plating multi-layer nano level metal or metal oxide, increase greatly the production cost of this material, cannot carry out suitability for industrialized production.
Summary of the invention
Object of the present invention is intended to for the multistage sliding sleeve of oil and gas reservoir staged fracturing build the pressure technical deficiency and the defect in ball material field, propose that a kind of reasonable mixture ratio of components, production technique are simple, the nucleocapsid structure formula magnesium alloy that can effectively decompose and preparation method thereof, make the decomposability of magnesium alloy surpass existing ingot metallurgy type magnesium alloy.
The invention provides a kind of magnesium alloy, by following component, by mass percent, formed: Al:5～24%, Fe:0.05～10%, Zn:0.2～5%, Zr:0.1～0.7%, Mn:0～0.2%, surplus is Mg, each component sum is 100%.
In the present invention, preferred described magnesium alloy is nucleocapsid structure formula magnesium alloy.More preferably, nucleome containing element magnesium, zinc and the zirconium of described magnesium alloy, the shell of described magnesium alloy is elementary composition by aluminium and two kinds of iron; Further, the nucleome of preferred described magnesium alloy is elementary composition or elementary composition by magnesium, aluminium, zinc, zirconium and five kinds, manganese by magnesium, zinc and three kinds of zirconiums.
The present invention also provides the application that build the pressure in ball material of described magnesium alloy in oil-gas mining.
The present invention also provides the preparation method of described magnesium alloy, comprise, steps A, batching and ball milling are coated: adopt spherical magnesium alloy and pure magnesium to be mixed with nucleome composite powder, adopt the metal powder preparation shell composite powder containing aluminium and iron content, nucleome composite powder is mixed with shell composite powder and carry out high-energy ball milling and be coated; Step B, moulding and sintering: the powder after the ball milling of steps A gained is coated adopts mold pressing form to be pressed into base substrate, and gained base substrate is carried out to sintering, obtains described nucleocapsid structure formula magnesium alloy.In the present invention, can prepare nucleome composite powder or shell composite powder by V-type machine or ball mill mixing powder raw material.
In above-mentioned preparation method, preferably, adopt fine aluminium and ferroaluminium to be mixed with shell composite powder.In preferred described nucleome composite powder, the mass ratio of spherical magnesium alloy powder and pure magnesium powder is 19:1～1:1, and in described shell composite powder, the mass ratio of pure aluminium powder and ferroaluminium powder is 4:1～1:2.
In preparation method of the present invention, preferably described spherical magnesium alloy is Mg-Al-Zn-Mn series magnesium alloy or Mg-Zn-Zr series magnesium alloy.
In embodiment of the present invention, the mass ratio of described nucleome composite powder and shell composite powder is 19:1～2:1.
Preferably, in high-energy ball milling of the present invention is coated, drum's speed of rotation is 300～600 revs/min, adopts argon shield; Described sintering carries out in vacuum sintering funace, and sintering temperature is 500～600 ℃, and during sintering, institute's applied pressure is 5～25MPa, sintering time 2～6h.During sintering, institute's applied pressure is provided by the hydraulic pulldown on blank top, by the compacting of powder blank.
Compared with prior art, the present invention by high-energy ball milling at nucleome powder surface encasement layer material, then pass through vacuum heating-press sintering, obtain the sintered state sample that density is high, hole is few, crystal grain is tiny, intermetallic compound small and dispersed distributes, make alloy structure in nucleocapsid structure formula state, thereby there is good comprehensive mechanical performance; Meanwhile, the decomposability of alloy in high temperature halogen solution obviously surpasses existing as-cast magnesium alloy.
Embodiment
In following comparative example and embodiment, in alloy composition, data represent its quality percentage composition; As the content of Al, Zn, Zr and Mn in AZ91 as-cast magnesium alloy Mg-9Al-0.9Zn-0.5Zr-0.2Mn is respectively 9%, 0.9%, 0.5% and 0.2%, surplus is Mg, totally 100%.
Comparative example 1
This comparative alloy is AZ91 as-cast magnesium alloy, and its chemical composition is Mg-9Al-0.9Zn-0.5Zr-0.2Mn.The raw material of AZ91 comprises A00 fine aluminium, Al-4Zr master alloy, No. 2 pure magnesiums, Al-10Mn master alloy and No. 2 pure zinc; Above-mentioned raw materials melting in Medium frequency induction resistance furnace, and use C
2cl
6carry out refining processing, through standing, skim, by swage, be cast into billet.The maximum incompressible intensity of room temperature of this alloy is 245MPa, and its erosion rate in the 3%KCl solution of 93 ℃ is 0.01g/h.
Comparative example 2
This comparative alloy is ZK61 as-cast magnesium alloy, and its chemical composition is Mg-6Zn-0.9Zr.The raw material of ZK61 comprises Mg-10Zr master alloy, No. 2 pure magnesiums and No. 2 pure zinc; Above-mentioned raw materials melting in Medium frequency induction resistance furnace, and use C
2cl
6carry out refining processing, through standing, skim, by swage, be cast into billet.The maximum incompressible intensity of room temperature of this alloy is 252MPa, and its erosion rate in the 3%KCl solution of 93 ℃ is 0.014g/h.
Embodiment 1
The alloy composition preparing in the present embodiment is: Mg-14.0Al-2.50Fe-0.65Zn-0.36Zr-0.14Mn.Its raw material comprises the spherical AZ91 magnesium alloy of-200 object powder ,-50 object Mg powder ,-50 object Al-50Fe powder and-300 object Al powder.The preparation method of this alloy is: the AZ91 powder and the pure magnesium powder that mass ratio, are first 4:1 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 1:1 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 9:1, under argon shield, by the rotating speed high-energy ball millings of 600 revs/min, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 550 ℃, and sintering time is 4h.The maximum incompressible intensity >=310MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.81g/h.
Embodiment 2
The alloy composition preparing in the present embodiment is: Mg-12.6Al-0.5Fe-0.81Zn-0.45Zr-0.18Mn.Its raw material comprises the spherical AZ91 magnesium alloy of-50 object powder ,-300 object Mg powder ,-300 object Al-50Fe powder and-50 object Al powder.The preparation method of this alloy is: the AZ91 powder and the pure magnesium powder that mass ratio, are first 19:1 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 4:1 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 19:1, under argon shield, by the rotating speed high-energy ball millings of 300 revs/min, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 500 ℃, and sintering time is 6h.The maximum incompressible intensity >=300MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.73g/h.
Embodiment 3
The alloy composition preparing in the present embodiment is: Mg-13.4Al-0.95Fe-0.77Zn-0.43Zr-0.17Mn.Its raw material comprises the spherical AZ91 magnesium alloy of-150 object powder ,-150 object Mg powder ,-150 object Al-50Fe powder and-150 object Al powder.The preparation method of this alloy is: the AZ91 powder and the pure magnesium powder that mass ratio, are first 11:1 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 2.5:1 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 14:1, under argon shield, by 450 revs/min of rotating speed ball millings, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 600 ℃, and sintering time is 2h.The maximum incompressible intensity >=310MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.76g/h.
Embodiment 4
The alloy composition preparing in the present embodiment is: Mg-23.2Al-10.0Fe-0.32Zn-0.18Zr-0.07Mn.Its raw material comprises the spherical AZ91 magnesium alloy of-200 object powder ,-50 object Mg powder ,-200 object Al-50Fe powder and-300 object Al powder.The preparation method of this alloy is: the AZ91 powder and the pure magnesium powder that mass ratio, are first 1:1 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 1:2 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 7:3, under argon shield, by 450 revs/min of rotating speed ball millings, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 600 ℃, and sintering time is 2h.The maximum incompressible intensity >=340MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.94g/h.
Embodiment 5
The alloy composition preparing in the present embodiment is: Mg-19.5Al-5.0Fe-0.45Zn-0.25Zr-0.10Mn.Its raw material comprises the spherical AZ91 magnesium alloy of-200 object powder ,-50 object Mg powder ,-200 object Al-50Fe powder and-300 object Al powder.The preparation method of this alloy is: the AZ91 powder and the pure magnesium powder that mass ratio, are first 5:3 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 1:1 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 4:1, under argon shield, by 400 revs/min of rotating speed ball millings, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 540 ℃, and sintering time is 4h.The maximum incompressible intensity >=320MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.85g/h.
Embodiment 6
The alloy composition preparing in the present embodiment is: Mg-10.0Al-5.0Fe-2.7Zn-0.41Zr.Its raw material comprises the spherical ZK61 magnesium alloy of-200 object powder ,-50 object Mg powder ,-200 object Al-50Fe powder and-300 object Al powder.The preparation method of this alloy is: the ZK61 powder and the pure magnesium powder that mass ratio, are first 9:8 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 1:2 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 17:3, under argon shield, by 400 revs/min of rotating speed ball millings, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 550 ℃, and sintering time is 4h.The maximum incompressible intensity >=300MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.78g/h.
Embodiment 7
The alloy composition preparing in the present embodiment is: Mg-5.2Al-1.04Fe-4.69Zn-0.70Zr.Its raw material comprises the spherical ZK61 magnesium alloy of-200 object powder ,-100 object Mg powder ,-200 object Al-50Fe powder and-200 object Al powder.The preparation method of this alloy is: the ZK61 powder and the pure magnesium powder that mass ratio, are first 5:1 are mixed with nucleation volume recombination powder with V-type machine, and the Al powder that is 2:1 mass ratio is mixed with into shell composite powder with Al-50Fe powder with V-type machine; Then getting mass ratio is nucleome powder and the shell powder of 15:1, under argon shield, by 400 revs/min of rotating speed ball millings, mixes; Then at room temperature compression molding; Pressed compact is sintering in vacuum sintering furnace, and sintering temperature is 550 ℃, and sintering time is 4h.The maximum incompressible intensity >=300MPa of room temperature of the alloy preparing with the method, its erosion rate in the 3%KCl solution of 93 ℃ is 0.65g/h.
Reasonable mixture ratio of components of the present invention, production technique are simple, can effectively improve bulk strength and the decomposability energy of magnesium alloy.Adopt nucleocapsid structure formula material, by the method for high-energy ball milling and vacuum heating-press sintering, obtain the tiny powder metallurgy magnesium alloy of crystal grain, make its performance meet oil and gas exploitation with building the pressure the requirement of ball to the intensity of material and decomposability; Expanded the application of magnesium alloy in oil and gas exploitation field, the powder metallurgy magnesium alloy that formation can practical application in industry.
Claims (10)
1. a magnesium alloy, is comprised of by mass percent following component:
Al:5～24%, Fe:0.05～10%, Zn:0.2～5%, Zr:0.1～0.7%, Mn:0～0.2%, surplus is Mg, each component sum is 100%.
2. magnesium alloy according to claim 1, is characterized in that, described magnesium alloy is nucleocapsid structure formula magnesium alloy.
3. magnesium alloy according to claim 2, is characterized in that, nucleome containing element magnesium, zinc and the zirconium of described magnesium alloy,
The shell of described magnesium alloy is elementary composition by aluminium and two kinds of iron; The nucleome of preferred described magnesium alloy is elementary composition or elementary composition by magnesium, aluminium, zinc, zirconium and five kinds, manganese by magnesium, zinc and three kinds of zirconiums.
One kind as described in any one in claim 1～3 magnesium alloy in the application building the pressure in ball material of oil-gas mining.
5. a preparation method for magnesium alloy as described in claim 2 or 3, comprises,
Steps A, batching and ball milling are coated: adopt spherical magnesium alloy and pure magnesium to be mixed with nucleome composite powder, adopt the metal powder preparation shell composite powder that contains aluminium and iron content, described nucleome composite powder is mixed with shell composite powder and carry out high-energy ball milling and be coated;
Step B, moulding and sintering: the powder after the ball milling of steps A gained is coated adopts mold pressing form to be pressed into base substrate, and gained base substrate is carried out to sintering, obtains described nucleocapsid structure formula magnesium alloy.
6. preparation method according to claim 5, is characterized in that, adopts fine aluminium and ferroaluminium to be mixed with shell composite powder.
7. preparation method according to claim 6, is characterized in that, in described nucleome composite powder, the mass ratio of spherical magnesium alloy powder and pure magnesium powder is 19:1～1:1, and in described shell composite powder, the mass ratio of pure aluminium powder and ferroaluminium powder is 4:1～1:2.
8. preparation method according to claim 5, is characterized in that, described spherical magnesium alloy is Mg-Al-Zn-Mn series magnesium alloy or Mg-Zn-Zr series magnesium alloy.
9. according to the preparation method described in any one in claim 5～8, it is characterized in that, the mass ratio of described nucleome composite powder and shell composite powder is 19:1～2:1.
10. according to the preparation method described in any one in claim 5～8, it is characterized in that, during described high-energy ball milling is coated, drum's speed of rotation is 300～600 revs/min, adopts argon shield; Described sintering carries out in vacuum sintering funace, and sintering temperature is 500～600 ℃, and during sintering, institute's applied pressure is 5～25MPa, sintering time 2～6h.
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| CN105618738A (en) * | 2016-03-17 | 2016-06-01 | 成都创源油气技术开发有限公司 | Method for manufacturing soluble tripping ball used for staged fracturing of shale gas well |
| CN105735959A (en) * | 2016-03-17 | 2016-07-06 | 成都创源油气技术开发有限公司 | Dissoluble tripping ball used for staged fracturing of shale gas well |
| CN105804715A (en) * | 2016-03-17 | 2016-07-27 | 成都创源油气技术开发有限公司 | Tripping ball for shale gas well fracturing |
| CN106854723A (en) * | 2016-12-09 | 2017-06-16 | 李晓光 | A kind of high plastic magnesium alloy at room temperature |
| CN107385245A (en) * | 2017-06-09 | 2017-11-24 | 西安理工大学 | Manufacture method based on oil-gas mining with soluble alloy pressure break ball |
| CN108179337A (en) * | 2017-12-25 | 2018-06-19 | 广东省材料与加工研究所 | The diecast magnesium alloy and its pressure casting method of a kind of high temperature creep-resisting |
| CN111304511A (en) * | 2020-03-27 | 2020-06-19 | 有研工程技术研究院有限公司 | Magnesium alloy material for oil and gas exploitation and preparation method and application thereof |
| CN114733454A (en) * | 2016-09-09 | 2022-07-12 | 流体力学与摩擦公司 | Multimaterial powder with composite particles for additive synthesis |
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| CN106854723A (en) * | 2016-12-09 | 2017-06-16 | 李晓光 | A kind of high plastic magnesium alloy at room temperature |
| CN107385245A (en) * | 2017-06-09 | 2017-11-24 | 西安理工大学 | Manufacture method based on oil-gas mining with soluble alloy pressure break ball |
| CN108179337A (en) * | 2017-12-25 | 2018-06-19 | 广东省材料与加工研究所 | The diecast magnesium alloy and its pressure casting method of a kind of high temperature creep-resisting |
| CN108179337B (en) * | 2017-12-25 | 2019-04-23 | 广东省材料与加工研究所 | A kind of diecast magnesium alloy and its pressure casting method of high temperature creep-resisting |
| CN111304511A (en) * | 2020-03-27 | 2020-06-19 | 有研工程技术研究院有限公司 | Magnesium alloy material for oil and gas exploitation and preparation method and application thereof |
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