CN106868368B - A kind of degradable magnesium alloy downhole tool sealing ball material and preparation method thereof - Google Patents
A kind of degradable magnesium alloy downhole tool sealing ball material and preparation method thereof Download PDFInfo
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- CN106868368B CN106868368B CN201710089825.9A CN201710089825A CN106868368B CN 106868368 B CN106868368 B CN 106868368B CN 201710089825 A CN201710089825 A CN 201710089825A CN 106868368 B CN106868368 B CN 106868368B
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- downhole tool
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- degradable magnesium
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007789 sealing Methods 0.000 title claims abstract description 14
- 239000011777 magnesium Substances 0.000 claims abstract description 35
- 239000000956 alloy Substances 0.000 claims abstract description 25
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 22
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005266 casting Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000010276 construction Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 23
- 239000011575 calcium Substances 0.000 claims description 22
- 239000011572 manganese Substances 0.000 claims description 19
- 238000005070 sampling Methods 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 238000007670 refining Methods 0.000 claims description 15
- 229910052788 barium Inorganic materials 0.000 claims description 14
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 14
- 230000004907 flux Effects 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 11
- 229910020091 MgCa Inorganic materials 0.000 claims description 10
- 229910017916 MgMn Inorganic materials 0.000 claims description 10
- 101100003996 Mus musculus Atrn gene Proteins 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 238000005275 alloying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 239000011701 zinc Substances 0.000 claims description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000000155 melt Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract 1
- 238000009472 formulation Methods 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- 238000007792 addition Methods 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 4
- 229910001626 barium chloride Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 241001074085 Scophthalmus aquosus Species 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- 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
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
- E21B33/134—Bridging plugs
-
- 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
- E21B34/00—Valve arrangements for boreholes or wells
- E21B34/06—Valve arrangements for boreholes or wells in wells
- E21B34/14—Valve arrangements for boreholes or wells in wells operated by movement of tools, e.g. sleeve valves operated by pistons or wire line tools
Landscapes
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Geochemistry & Mineralogy (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to degradable magnesium alloy field of material preparation, is developed for oil gas field field, specifically discloses a kind of degradable magnesium alloy downhole tool sealing ball material and preparation method thereof.According to component design ratio Zn, Mn, Ca, Mg metal is weighed prepare by technique, obtained ingot casting be processed into it is cylindric after subject alloy material, specified structure form is then processed into by the material.According to magnesium alloy made from inventive formulation and technique, crystal habit is good, mechanical strength is high, can be dissolved in the solution containing electrolyte, pressing crack construction instrument is manufactured using solvable magnesium alloy, instrument voluntarily melts after task is completed in underground, then mixes and is discharged in a liquid by the way that pipeline is counter, can be degradable, in the absence of easy bite, blocking channel problem, mill recovery process is bored so as to save, engineering difficulty is reduced, improves efficiency of construction.
Description
Technical field
The invention belongs to degradable magnesium alloy field of material preparation, specially a kind of degradable magnesium alloy downhole tool sealing
Ball material and preparation method thereof.
Background technology
Chinese Low Permeability Oil/gas aboundresources, there is very big exploration-development potential.In recent decades, in hyposmosis sand
Very big discovery is achieved in terms of rock, Marine Carbonate Rocks, volcanic rock exploration, forms world-class exploitation supporting technology.
Low permeability oil and gas field exploitation mature technology has water filling, pressure break, gas injection etc..
The stable yields of following oil and gas production, volume increase will rely more heavily on these hyposmosis unconventional petroleum resourceses.Oil gas provides
Source is distributed in the stratum of different depth mostly, can be realized using multilayer multistage fracturing technique and meanwhile the transformation to multiple stratum come
Single well productivity is improved, so as to improve efficiency of construction.
The reservoir reconstruction technologies such as hydraulic fracturing, acid fracturing must be relied on by developing these unconventional petroleum resourceses, wherein adopting
The multilayer multistage pressure break carried out with downhole tool is a technology being commonly used.
In multilayer multistage pressure break, need to use isolating tool between interval（Such as pressure break ball, bridging plug）Pressure break is successively carried out after separation
Transformation, treat that isolating tool is returned into discharge pit shaft again after the completion of all interval constructions, to get through the exploitation that hoistway realizes oil, gas.
At present, commonly use isolating tool to be made by steel mostly, brill milling difficulty be present, time-consuming, powder, fragment are not easy after brill
The shortcomings of row of returning.
It is difficult to there is the row of returning because than great in the ferrous materials as the first generation；Second generation composite, although solving
Heavy problem, but because can not be degradable, easy bite, blocking channel problem, and raw material production be present and add
Work need to rely on import, somewhat expensive；Can not be degradable during underground mining, the characteristics of easy bite be present.
And the application aims to provide third generation degradation material, field of petroleum exploitation is can be widely used for, has and surmounts second
, can be degradable for material property, in the absence of easy bite, blocking channel problem, and production cost can be reduced, be used primarily in well
In the submount material processing component assembly of lower instrument.
The content of the invention
The purpose of the present invention is to be directed to problem above, there is provided a kind of degradable magnesium alloy downhole tool sealing ball material and its
Preparation method, pressing crack construction instrument being manufactured using solvable magnesium alloy, instrument voluntarily melts after task is completed in underground,
Then mix and discharged in a liquid by the way that pipeline is counter, can be degradable, in the absence of easy bite, blocking channel problem, bored so as to save
Recovery process is ground, reduces engineering difficulty, improves efficiency of construction.
To realize object above, the technical solution adopted by the present invention is：A kind of degradable magnesium alloy downhole tool ball sealer
The mass fraction content of material, the degradable magnesium alloy downhole tool submount material constituent and each composition is as follows：
A kind of degradable magnesium alloy downhole tool seals ball material, it is characterised in that degradable magnesium alloy underground work
The mass fraction content for having submount material constituent and each composition is as follows：
Zinc（Zn）：17%-21%；
Manganese（Mn）：0.6%-1.0%；
Calcium（Ca）：0.6%-1.0%；
Surplus is magnesium（Mg）, above each component mass fraction sum is 100%.
Preferably, the degradable magnesium alloy downhole tool submount material is used to produce the pressure break during exploitation of oil-gas field
Construction use can melt ball sealer.
Another technical scheme of the present invention, formula and a kind of degradable magnesium alloy downhole tool ball sealer of component more than
The preparation method of material, comprises the following steps：
（1）Melting prepares：Crucible internal washing is clean, hang in resistance furnace, open electric furnace, heated to crucible dark red
Color, surface sprinkle barium fluxing agent；
（2）Charging refining：Example prepares raw material in mass ratio, and charging sequence is as follows：It is uniformly added into magnesium ingot to be allowed to melt, metal
Zn materials can add with magnesium ingot, and Mn, Ca material first make MgMn, MgCa alloy material with Mg, then be placed on table pre-
Heat, temperature reach 750 DEG C or so addition MgMn alloy materials, and temperature reaches 780 DEG C of addition MgCa alloy materials, and uniform stirring makes
Solution alloying；
（3）Centre sampling：Sampling detection chemical composition, qualified rear seal-cover stand about one hour；
（4）Casting rod is molded：Treat step（2）After middle sampling is qualified, direct chill casting is used at 740 DEG C into casting rod；
（5）Material tests：Sampling detection chemical composition, mechanical property, metallographic structure, test corrosion rate after stove.
Preferably, in step（2）Feed in refining process, the process of haveing suffered is sufficiently stirred liquation, and sheds barium fluxing agent and go out
Fire, make liquation alloying.
Preferably, in step（2）Feed in refining process, MgMn, MgCa alloy material are placed on when being preheated on table, are used
Thermocouple measurement melt temperature.
Preferably, in step（3）Before the sampling of centre, temperature refines at 760 DEG C, sheds No. six flux, uniform stirring makes conjunction
After golden liquid light, then it is sampled operation.
Preferably, step（2）Magnesium in charging refining（Mg）, zinc（Zn）, manganese（Mn）, calcium（Ca）The purity of metal >=
99.9%。
Preferably, step（1）During melting prepares, the temperature control of electric furnace heating crucible is at 690-780 DEG C.
Barium fluxing agent（RJ-2）It is the eutectic that the chloride high melt such as potassium chloride, magnesium chloride, barium chloride mixes,
Also a small amount of barium chloride calcination can be added by carnallite and magnesia or other methods synthesizes, closed available for magnesium alloy or magnalium
The productions containing magnesium alloy such as gold.During high melt magnesium metal, block magnesium is easily aoxidized and burnt, and when coming out of the stove, adds appropriate powder
Shape barium fluxing agent can prevent the burning of magnesium metal；In refined metals magnesium, add barium fluxing agent and refined, can be from fused solution
Oxide impurity and nitride are settled out, therefore barium fluxing agent can be used for the refining agent and protective agent of magnesium and magnesium alloy；In addition two
Number flux can be additionally used in magnesium alloy welding compound and metal fusing agent.The purposes of barium fluxing agent is different, wherein the content of each component
Also it is different, and the raw material of other impurities or remained unreacted may be introduced in fusion process, therefore need to be to barium fluxing agent
The content of middle magnesia is measured.
No. six flux（RJ-6）Be by the high melts such as potassium chloride, barium chloride, calcium chloride, calcirm-fluoride cast it is blocking, then
It is broken to wear into powdery by ball mill, turn into product after sieving；Addition potassium chloride can significantly reduce the fusing point of flux, surface tension
And viscosity, improve the stability of flux；Addition barium chloride can increase the density of flux, make flux and Serum Magnesium more easily separated；Fluorine
Change calcium and can not only be used for thickening agent use, can also improve the stability and affinability of flux；Because containing calcium in this material, and chlorine
Change magnesium and the compound of chemical reaction generation calcium chloride easily occurs with calcium, therefore select No. six flux of not magnesium chloride containing as refining
Agent.
Beneficial effects of the present invention：The invention provides a kind of degradable magnesium alloy downhole tool sealing ball material and its system
Preparation Method, pressing crack construction instrument is manufactured using solvable magnesium alloy, instrument voluntarily melts after task is completed in underground, so
Mix and discharged in a liquid by the way that pipeline is counter afterwards, can be degradable, in the absence of easy bite, blocking channel problem, mill is bored so as to save
Recovery process, engineering difficulty is reduced, improve efficiency of construction.
The present invention material, metal Zn materials and magnesium combination precipitation strength phase based on magnesium, improve alloy strength, improve and close
The tensile property of gold；It is mainly to improve the corrosion rate of alloy to improve content.Metal Mn materials mainly play obstruction and closed in the alloy
The big effect of Jin Jing's grain length, the yield strength of alloy is improved, improve alloy weldability.Metal Ca materials can improve the smelting of alloy
Golden amount, mitigate the oxidation during metal bath and heat treating castings；Refining alloy crystal grain, improve alloy creep drag.
Brief description of the drawings
Fig. 1 is cylinder casting rod product diameter circle centre position（0.5D, amplify 200 times）Metallograph.
Fig. 2 is at cylinder casting rod product diameter a quarter（0.25D, amplify 200 times）Metallograph.
Fig. 3 is material corrosion curve map.Scale is defined by left side coordinate at G lines in figure；Other scales are with the right coordinate
It is defined（The right coordinate value is 5 times of actual measured value, and corrosion rate is shown for amplifying）.
Fig. 4 is the mechanical property stress strain curve figure of material.
Supplementary notes：
The real composition proportioning of above metallograph is embodiment 1. Mg-18.5Zn-0.7Mn-0.7Ca；Embodiment 2. Mg-
20Zn-0.9Mn-0.9Ca metallograph is similar 1., therefore omits.
The corrosion rate of embodiment 1. is 12 mg/cm2.h, the corrosion rate of embodiment 2. is 15 mg/cm2.h。
1. tensile strength is 140.2MPa to embodiment, yield strength 101.8MPa, elongation percentage 1.2, and hardness is
73.6HBW；2. tensile strength is 138.5MPa to embodiment, yield strength 102.3MPa, elongation percentage 1.0, and hardness is
75.3HBW。
Real composition proportioning is 1. Mg-18.5Zn-0.7Mn-0.7Ca；Front-end digital is represented as mass fraction, i.e. Mg-
18.5Zn-0.7Mn-0.7Ca：Represent the Zn, 0.7% Mn, 0.7% Ca that mass fraction is 18.5%, surplus Mg, gross mass
Fraction is 100%.
Embodiment
In order that those skilled in the art more fully understand technical scheme, the present invention is entered below in conjunction with the accompanying drawings
Row is described in detail, and the description of this part is only exemplary and explanatory, should not there is any limitation to protection scope of the present invention
Effect.
Embodiment is 1.：
The present embodiment provides a kind of manufacture degradable magnesium alloy material, specific mass component：
Zn:18.5%,Mn:0.7%, Ca:0.7%, surplus Mg, above each component mass fraction add trace impurity sum
For 100%.
The preparation method of formula and a kind of degradable magnesium alloy downhole tool of component sealing ball material more than, including
Following steps：
（1）Melting prepares：Crucible internal washing is clean, hang in resistance furnace, open electric furnace, the temperature of electric furnace heating crucible
Degree control heats kermesinus at 690-730 DEG C, to crucible, and surface sprinkles barium fluxing agent；
（2）Charging refining：Example prepares raw material in mass ratio, and charging sequence is as follows：It is uniformly added into magnesium ingot to be allowed to melt, metal
Zn materials can add with magnesium ingot, and Mn, Ca material first make MgMn, MgCa alloy material with Mg, then be placed on table pre-
Heat, using thermocouple measurement melt temperature, temperature reaches 750 DEG C or so addition MgMn alloy materials, and temperature reaches 780 DEG C of additions
MgCa alloy materials, uniform stirring make solution alloying；The process of haveing suffered is sufficiently stirred liquation, and sheds barium fluxing agent fire extinguishing, makes
Liquation alloying；
（3）Centre sampling：Sampling detection chemical composition, qualified rear seal-cover stand about one hour；Temperature refines at 760 DEG C,
No. six flux are shed, after uniform stirring makes aluminium alloy light, then are sampled operation.
（4）Casting rod is molded：Treat step（2）After middle sampling is qualified, direct chill casting is used at 740 DEG C into casting rod；
（5）Material tests：Sampling detection chemical composition, mechanical property, metallographic structure, test corrosion rate after stove.
Preferably, step（2）Magnesium in charging refining（Mg）, zinc（Zn）, manganese（Mn）, calcium（Ca）The purity of metal >=
99.9%。
The performance and detection parameters of product are shown in accompanying drawing 1-4.
Embodiment is 2.：
The present embodiment provides a kind of manufacture degradable magnesium alloy material, specific mass component：
Zn:20.0%,Mn:0.9%, Ca:0.9%, surplus Mg, above each component mass fraction add the trace impurity sum to be
100%。
The preparation method of formula and a kind of degradable magnesium alloy downhole tool of component sealing ball material more than, including
Following steps：
（1）Melting prepares：Crucible internal washing is clean, hang in resistance furnace, open electric furnace, the temperature of electric furnace heating crucible
Degree control heats kermesinus at 690-780 DEG C, to crucible, and surface sprinkles barium fluxing agent；
（2）Charging refining：Example prepares raw material in mass ratio, and charging sequence is as follows：It is uniformly added into magnesium ingot to be allowed to melt, metal
Zn materials can add with magnesium ingot, and Mn, Ca material first make MgMn, MgCa alloy material with Mg, then be placed on table pre-
Heat, using thermocouple measurement melt temperature, temperature reaches 750 DEG C or so addition MgMn alloy materials, and temperature reaches 780 DEG C of additions
MgCa alloy materials, uniform stirring make solution alloying；The process of haveing suffered is sufficiently stirred liquation, and sheds barium fluxing agent fire extinguishing, makes
Liquation alloying；
（3）Centre sampling：Sampling detection chemical composition, qualified rear seal-cover stand about one hour；Temperature refines at 760 DEG C,
No. six flux are shed, after uniform stirring makes aluminium alloy light, then are sampled operation.
（4）Casting rod is molded：Treat step（2）After middle sampling is qualified, direct chill casting is used at 740 DEG C into casting rod；
（5）Material tests：Sampling detection chemical composition, mechanical property, metallographic structure, test corrosion rate after stove.
Preferably, step（2）Magnesium in charging refining（Mg）, zinc（Zn）, manganese（Mn）, calcium（Ca）The purity of metal >=
99.9%。
The performance and detection parameters of product are shown in accompanying drawing 3-4.
Pass through detection, product mechanical property tensile strength：More than 135MPa, yield strength：More than 100 MPa, elongation percentage：
More than 0.5%, Brinell hardness：More than 70HBW. corrosion rates：Material is in 3% Klorvess Liquid, 92 degree of constant temperature, corrodes 24 hours
Tried out, reduced than second generation cost, and performance and corrosive effect all conform to by client for 8-18mg/cm2.h. materials afterwards
Ask.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
And also include the other element being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to help the method and its core concept for understanding the present invention.Described above is only the preferred embodiment of the present invention, should
When pointing out, due to the finiteness of literal expression, for those skilled in the art, original of the invention is not being departed from
On the premise of reason, some improvement, retouching or change can also be made, above-mentioned technical characteristic can also be carried out by rights
Combination；These improve retouching, change or combination, or not improved the design of invention and technical scheme are directly applied into other fields
Close, be regarded as protection scope of the present invention.
Claims (7)
1. a kind of degradable magnesium alloy downhole tool seals ball material, it is characterised in that the degradable magnesium alloy downhole tool
Submount material constituent and the mass fraction content of each composition are as follows：
Zinc（Zn）：17%-21%；
Manganese（Mn）：0.6%-1.0%；
Calcium（Ca）：0.6%-1.0%；
Surplus is magnesium（Mg）, above each component mass fraction sum is 100%；
The degradable magnesium alloy downhole tool submount material can disappear for the pressing crack construction use during producing exploitation of oil-gas field
Melt ball sealer.
2. a kind of preparation method of degradable magnesium alloy downhole tool sealing ball material according to claim 1, its feature
It is, comprises the following steps：
（1）Melting prepares：Crucible internal washing is clean, hang in resistance furnace, open electric furnace, kermesinus, table are heated to crucible
Face sprinkles barium fluxing agent；
（2）Charging refining：Example prepares raw material in mass ratio, and charging sequence is as follows：It is uniformly added into magnesium ingot to be allowed to melt, metal Zn materials
Material can add with magnesium ingot, and Mn, Ca material first make MgMn, MgCa alloy material with Mg, are then placed on table and preheat, temperature
Degree reaches 750 DEG C or so addition MgMn alloy materials, and temperature reaches 780 DEG C of addition MgCa alloy materials, and uniform stirring makes solution
Alloying；
（3）Centre sampling：Sampling detection chemical composition, qualified rear seal-cover stand about one hour；
（4）Casting rod is molded：Treat step（2）After middle sampling is qualified, direct chill casting is used at 740 DEG C into casting rod；
（5）Material tests：Sampling detection chemical composition, mechanical property, metallographic structure, test corrosion rate after stove.
3. a kind of preparation method of degradable magnesium alloy downhole tool sealing ball material according to claim 2, its feature
It is, in step（2）Feed in refining process, whole process is sufficiently stirred liquation, and sheds barium fluxing agent fire extinguishing, makes liquation
Alloying.
4. a kind of preparation method of degradable magnesium alloy downhole tool sealing ball material according to claim 2, its feature
It is, in step（2）Feed in refining process, MgMn, MgCa alloy material are placed on when being preheated on table, using thermocouple measurement
Melt temperature.
5. sealing the preparation method of ball material according to a kind of degradable magnesium alloy downhole tool described in claim 2, its feature exists
In in step（3）Before the sampling of centre, temperature refines at 760 DEG C, sheds No. six flux, after uniform stirring makes aluminium alloy light, then
It is sampled operation.
6. sealing the preparation method of ball material according to a kind of degradable magnesium alloy downhole tool described in claim 2, it is characterised by,
Step（2）Magnesium in charging refining（Mg）, zinc（Zn）, manganese（Mn）, calcium（Ca）Purity >=99.9% of metal.
7. sealing the preparation method of ball material according to a kind of degradable magnesium alloy downhole tool described in claim 2, it is characterised by,
Step（1）During melting prepares, the temperature control of electric furnace heating crucible is at 690-780 DEG C.
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| CN107956462B (en) * | 2017-10-27 | 2020-09-08 | 中国石油天然气股份有限公司 | Downhole soluble tool and preparation method thereof |
| CA3039574A1 (en) * | 2018-05-10 | 2019-11-10 | Josh Caris | Degradable high-strength zinc compositions and method of manufacture |
| CN109406335A (en) * | 2018-10-26 | 2019-03-01 | 西南石油大学 | Bridge plug dissolution rate Lab-evaluation device and method under high temperature and high pressure environment |
| CA3174268A1 (en) | 2020-05-07 | 2021-11-11 | Shinnosuke Yoshida | Frac plug and method for manufacturing same, and method for sealing borehole |
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