CN108385108B - A kind of single crystal super alloy precision castings milling cream and its preparation method and application - Google Patents
A kind of single crystal super alloy precision castings milling cream and its preparation method and application Download PDFInfo
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- CN108385108B CN108385108B CN201810352161.5A CN201810352161A CN108385108B CN 108385108 B CN108385108 B CN 108385108B CN 201810352161 A CN201810352161 A CN 201810352161A CN 108385108 B CN108385108 B CN 108385108B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C23F1/14—Aqueous compositions
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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Abstract
A kind of single crystal super alloy precision castings milling cream and its preparation method and application, belongs to surface milling technical field.The single crystal super alloy precision castings milling cream is the mixture of mixed aqueous solution and positive compound of silicate class, by volume, mixed aqueous solution: positive compound of silicate class=1:(2~5)；In mixed aqueous solution: sulfuric acid is 9~18molL‑1, FeCl3For 0.3~2.0molL‑1, MnO2For 3.0~10.0gL‑1.Preparation method is to prepare mixed aqueous solution, and positive compound of silicate class is added and stirs 1~2h.It carries out milling to single crystal super alloy precision castings and testing piece, is particularly suitable for carrying out milling to single crystal super alloy precision castings local surfaces.The single crystal super alloy precision castings milling cream volatility is low, milling effect is good, it is relatively friendly to environment, it is mainly used for removing in casting technique that recrystallization defect in follow-up heat treatment process can be effectively reduced in single crystal super alloy precision castings part Plastic Deformation of Surface Layer residual stress concentrations layer.
Description
Technical field
The present invention relates to surface milling technical fields, and in particular to a kind of single crystal super alloy precision castings milling cream and its system
Preparation Method and application.
Background technique
Nickel base superalloy is a kind of high-temperature structural material using nickel as matrix, has very high room temperature intensity and high temperature strong
Degree, excellent creep and fatigue resistance, good anti-oxidant and hot corrosion resistance, good structure stability and use are reliable
Property.Nickel base superalloy is mainly used to manufacture the most thermal part of aero-jet engine and various industry gas turbines, such as whirlpool
Take turns guide vane, working-blade, the turbine disk etc. of part.It or rocket engine and gas turbine high temperature hot-end component are not
Alternative material.
In the latest 20 years, nickel base superalloy experienced several stages such as equiax crystal, directional columnargrain, single crystal alloy, hold height
Warm ability constantly enhances.Single crystal super alloy experienced the alloy without Re alloy to second generation 3%Re from the first generation, developing deeply
Alloy to the third generation containing 6%Re, and the forth generation of elements and the 5th Dai Hejin such as Ru, Ir are added on the basis of high Re.But
Single crystal alloy is during directional solidification casting precision castings, casting local surfaces, such as surface discontinuity position, casting construction mutation
Position etc. can generate it is larger be plastically deformed residual stress layer, residual stress is the inducement of the crystal grain defects such as recrystallization, then ties
Crystalline substance causes single crystal casting fatigue behaviour and creep rupture life performance to be remarkably decreased, and endangers monocrystalline precision castings huge.
Monocrystalline precision castings surface plastic deformation residual stress layer must remove.Milling is effective means.But current milling side
Method, which is all made of, to be directly immersed in precision castings in corrosive liquid or is not intended to the inner cavity of milling to be immersed in corruption again with sealing with wax precision castings
Lose the method for milling in liquid.The above method, which will lead to precision castings and not need the surface of milling, to be corroded, and sealing with wax not can avoid yet.This
It will lead to precision castings performance and service life reduction.
In addition, existing milling agent have the shortcomings that pollute Environmental insults endanger it is big.It is found through the Searches of Patent Literature, it is Ni-based
The patent of high temperature alloy milling mostly uses greatly reagent unfriendly to environment, seriously polluted.Such as patent CN101696501A is mentioned
A kind of gone out high-temperature alloy blades finish forge chemical milling solution and milling method, using the hydrochloric acid of 55-75g/L, 100-135g/L
The ferric chloride aqueous solutions of nitric acid and 400-500g/L, this corrosive agent can also be to first generation single crystal super alloys
Milling.For contain the Re second generation, third generation nickel-base high-temperature single crystal alloy, patent CN103451657A using 200-400mL nitric acid,
150-350mL hydrofluoric acid, 350-700mL distilled water, 20-60 DEG C, corrosion 90-200min can effectively remove plastic deformation layer.Specially
Sharp CN102330087A uses the concentration of hydrochloric acid for 220~300mL/L, and the concentration of hydrofluoric acid is 200~300mL/L, nitric acid
Concentration is 110~120mL/L, and the concentration of acetic acid is 40~45mL/L, and the concentration of ferric trichloride is 300~350g/L, chromic anhydride
Concentration is that 18~21g/L makees milling agent.In these chemical milling methods, hydrochloric acid is volatility acid very serious, and hydrofluoric acid is to ring
Border and human body damage acid very serious, and chromic anhydride will become carcinogen and do great harm to human body under the conditions of acid with strong oxidizing property.
Therefore, researching and developing a kind of can seem especially heavy to the environmental-friendly chemical milling method of single crystal super alloy precision castings local surfaces
It wants.
Summary of the invention
The object of the present invention is to provide a kind of single crystal super alloy precision castings milling cream and its preparation method and application, the lists
Brilliant high temperature alloy precision castings milling cream volatility is low, and milling effect is good, relatively friendly to environment, can be applied to precision castings part
Realize the milling of precision castings part in surface.The application of the single crystal super alloy precision castings milling cream is mainly used for removing founder
In single crystal super alloy precision castings part Plastic Deformation of Surface Layer residual stress concentrations layer in skill, subsequent heat treatment mistake can be effectively reduced
Recrystallization defect in journey.
A kind of single crystal super alloy precision castings milling cream of the invention, including sulfuric acid, FeCl3、MnO2, water and positive esters of silicon acis
Class compound；It wherein, is the mixed of mixed aqueous solution and positive compound of silicate class in single crystal super alloy precision castings milling cream
It closes, by volume, mixed aqueous solution: positive compound of silicate class=1:(2~5)；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 9~18molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration be 0.3~
2.0mol·L-1, MnO2Mass concentration is 3.0~10.0gL-1, surplus is water.
The positive compound of silicate class is methyl orthosilicate, in ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate
One or more of mixing, mixed proportion is any ratio.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, by sulfuric acid, FeCl3And MnO2Mixing, stirs evenly, obtains sulfuric acid, FeCl3And MnO2's
Aqueous solution；
Step 2: mixing
According to the ratio, positive compound of silicate class is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, be stirred at room temperature 1~
Single crystal super alloy precision castings milling cream is made in 2h.
In the step 2, the stirring, stirring rate is 30~60 turns/min.
A kind of application of single crystal super alloy precision castings milling cream, to carry out milling, tool to single crystal super alloy precision castings
Body sequentially includes the following steps:
(1) prepare
Handle single crystal super alloy precision castings: the surface impurity of cleaning single crystal super alloy precision castings, after obtaining pretreatment
Single crystal super alloy precision castings；
It prepares milling cream: according to the ratio, weighing raw material, prepare single crystal super alloy precision castings milling cream；
(2) by milling cream be applied to pretreated single crystal super alloy precision castings residual stress concentrations local surfaces and
In testing piece known to thickness, testing piece known to pretreated single crystal super alloy precision castings and thickness is made uniformly to smear thickness
Spend 2-3mm milling cream, will apply wipe testing piece known to the single crystal super alloy precision castings and thickness of milling cream be heated to 30~
60 DEG C, corrode 90~200min, the testing piece after single crystal super alloy precision castings and corrosion after being corroded；
(3) after the milling cream of the single crystal super alloy precision castings after corrosion and the testing piece surface after corrosion being wiped, into
Row cleaned by ultrasonic vibration, removal residual corrosion product, then be rinsed with water, it dries, according to the thickness change of testing piece, determines single
The removal amount of brilliant high temperature alloy precision castings；
(4) when removal amount is unsatisfactory for application request or cannot completely remove surface plastic deformation layer, then repeatedly step
(2) and (3), until reaching application request.
In the step (1), the single crystal super alloy precision castings are nickel-base high-temperature single crystal alloy precision castings.
In the nickel-base high-temperature single crystal alloy precision castings, the mass percent of the ingredient and each ingredient that contain is that C is
0.03%~0.075%, Cr be 6.5%~7.3%, Co be 7%~8%, W be 4.75%~5.25%, Mo be l.3%~
1.7%, Ta are that 6.5%~6.7%, A1 is 5.8%~6.4%, Y < 0.03%, surplus Ni.
In the step (2), the testing piece is the list prepared using identical preparation process and same alloy ingredient
Brilliant high temperature alloy testing piece.
In the step (2), corrosion process will carry out in constant temperature field, and temperature fluctuation range is ± 1 DEG C.
In the step (3), in cleaned by ultrasonic vibration, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle.
In the step (3), in the aqueous solution containing nano-alpha aluminium oxide particle, nano-alpha aluminium oxide particle grain
Diameter is 50~300nm, and the mass concentration of alpha aluminium oxide particle is 0.1~2.0gL-1, aqueous temperature is room temperature, aqueous solution pH
Value is 7 ± 0.1.
In the step (3), the ultrasonic frequency is in 10~80kHz.
In the step (3), the ultrasonic cleaning time is 30~90min.
The application of the single crystal super alloy precision castings milling cream, is particularly suitable for single crystal super alloy precision castings office
Portion surface carries out milling.
The present invention provides a kind of single crystal super alloy precision castings milling cream and its preparation method and application, has following excellent
Point:
1, the present invention has environmentally friendly, easy to operate, manageable feature.
2, the residual stress layer on part removal single crystal super alloy surface layer can be achieved in the present invention, reduces and ties again caused by deformation
Brilliant defect increases the yield rate of single crystal super alloy precision castings.
3, the present invention can show the grain structure of single crystal alloy simultaneously.
4, the present invention solves asking for single crystal super alloy precision castings part milling using the milling cream for preparing paste body shape
Topic, during preparing single crystal super alloy precision castings milling cream, raw material can will be changed by hydrolysis, condensation, the lotion of preparation
Milling active constituent effectively adequately disperses, is adsorbed in single crystal super alloy precision castings milling cream, to realize to monocrystalline high temperature
Alloy precision castings carry out milling.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, remove specified otherwise, the raw material and equipment of use be it is commercially available, the purity of raw material be analyze it is pure and
More than.
Embodiment 1
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 9molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.3molL-1,
MnO2Mass concentration is 3.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream, to carry out milling, tool to single crystal super alloy precision castings
Body sequentially includes the following steps:
(1) prepare
Processing single crystal super alloy precision castings: cleaning the surface impurity of nickel-base high-temperature single crystal alloy precision castings to be milled,
Obtain pretreated nickel-base high-temperature single crystal alloy precision castings；Wherein, in the nickel-base high-temperature single crystal alloy precision castings, contain
Ingredient and each ingredient mass percent be C be 0.03%~0.075%, Cr be 6.5%~7.3%, Co be 7%~
8%, W be 4.75%~5.25%, Mo be l.3%~1.7%, Ta be 6.5%~6.7%, A1 be 5.8%~6.4%, Y <
0.03%, surplus Ni.
It prepares milling cream: according to the ratio, weighing deionized water, ethyl orthosilicate, the concentrated sulfuric acid, FeCl3.6H2O, MnO2, prepare
Sulfuric acid concentration is 9molL-1, FeCl3Concentration is 0.3molL-1, MnO2Content is 3.0gL-1Mixed aqueous solution, will mix
Heshui solution and ethyl orthosilicate are matched according to volume ratio 1:3, are 30 turns/min in revolution, are stirred 1h under room temperature and are formed
Cream.
(2) by milling cream be applied to pretreated single crystal super alloy precision castings part residual stress concentrations surface and
In testing piece known to thickness, keep testing piece known to pretreated single crystal super alloy precision castings local surfaces and thickness equal
Even smearing thickness 2-3mm milling cream is heated to 40 ± 1 DEG C using water-bath, corrodes 90min, the nickel-based monocrystal after being corroded
Testing piece after high temperature alloy precision castings and corrosion；
The testing piece is to use preparation process identical with nickel-base high-temperature single crystal alloy precision castings and same alloy ingredient
The single crystal super alloy testing piece of preparation.
(3) by the milling on the testing piece surface after the nickel-base high-temperature single crystal alloy precision castings local surfaces and corrosion after corrosion
After cream erasing, cleaned by ultrasonic vibration 30min, removal residual corrosion product are carried out in the ultrasonic wave that frequency is 10kHz, then use
Water rinses, and dries, reduces by 2.8 μm, under this condition, nickel-based monocrystal altogether with the thickness of high-precision digital-display miking testing piece
The removal amount of high temperature alloy precision castings is about 2.7 μ m-thicks, meets application request.
In cleaned by ultrasonic vibration, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, wherein nano-alpha aluminium oxide
Grain diameter is 50~300nm, and the mass concentration of alpha aluminium oxide particle is 0.1-2.0gL-1, aqueous temperature is room temperature, water
Solution ph is 7.
Embodiment 2
A kind of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 1, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 2.6 μm altogether, and under this condition, DD32 essence casting blade surface is about
Eliminate 2.5 μ m-thicks.
Other modes are identical.
Embodiment 3
A kind of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 1, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 2.5 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 1.7 μ m-thicks.
Other modes are identical.
Embodiment 4
A kind of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 1.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 1, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 1.7 μm altogether, and under this condition, DD6 essence casting blade surface is divided out
In addition to 1.6 μ m-thicks.
Other modes are identical.
Embodiment 5
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 10molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.4molL-1,
MnO2Mass concentration is 3.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 10molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 0.4molL-1, MnO2Content is 3.0g
L-1Mixed aqueous solution, 1:3 is prepared by volume for mixed aqueous solution and ethyl orthosilicate, is stirred in the case where revolution is 30 turns/min room temperature
It mixes mixing 1h and forms cream；
(2) milling etching time 120min；
For C0.03~0.075%, Cr6.5~7.3%, Co7~8%, W4.75~5.25%, Mol.3~1.7%,
Ta6.5~6.7%, A15.8~6.4%, Y < 0.03%, surplus are the nickel-base high-temperature single crystal alloy precision castings of Ni and same with technique
The single crystal super alloy testing piece milling of ingredient preparation, the thickness of single crystal super alloy testing piece reduces 12 μm altogether, in the condition
Under, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 11 μ m-thicks.
Embodiment 6
A kind of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 5, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 9 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 8.6 μ m-thicks.
Other modes are identical.
Embodiment 7
A kind of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 5, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 9.5 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 9 μ m-thicks.
Other modes are identical.
Embodiment 8
A kind of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 5.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 5, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 9 μm altogether, and under this condition, DD6 essence casting blade surface about removes
8.5 μ m-thicks.
Other modes are identical.
Embodiment 9
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 11molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.5molL-1,
MnO2Mass concentration is 3.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 11molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 0.5molL-1, MnO2Content is 3.0g
L-1Aqueous solution and ethyl orthosilicate by volume 1:3 prepare, revolution be 30 turns/min room temperature under be stirred 1h formed cream；
(2) milling etching time 180min；
It is 0.03~0.075%, Cr for C be 6.5~7.3%, Co be 7~8%, W is that 4.75~5.25%, Mo is
L.3~1.7%, Ta is that 6.5~6.7%, A1 is 5.8~6.4%, Y < 0.03%, and surplus is the nickel-base high-temperature single crystal alloy of Ni
Precision castings and single crystal super alloy testing piece milling with the congruent preparation of technique, the thickness of single crystal super alloy testing piece subtract altogether
24 μm few, under this condition, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 23 μ m-thicks.
Embodiment 10
A kind of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 9, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 22 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 21.5 μ m-thicks.
Other modes are identical.
Embodiment 11
A kind of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 9, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 22 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 21 μ m-thicks.
Other modes are identical.
Embodiment 12
A kind of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 9.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 9, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 22 μm altogether, and under this condition, DD6 essence casting blade surface is divided out
In addition to 21 μ m-thicks.
Other modes are identical.
Embodiment 13
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 11molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.6molL-1,
MnO2Mass concentration is 3.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 11molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 0.6molL-1, MnO2Content is 3.0g
L-1Aqueous solution and ethyl orthosilicate by volume 1:3 prepare, revolution be 30 turns/min room temperature under be stirred 1h formed cream；
(2) milling etching time 180min；
It is 0.03~0.075%, Cr my 6.5~7.3%, Co for C be 7~8%, W is that 4.75~5.25%, Mo is
L.3~1.7%, Ta is that 6.5~6.7%, A1 is 5.8~6.4%, Y < 0.03%, and surplus is the nickel-base high-temperature single crystal alloy of Ni
Precision castings and single crystal super alloy testing piece milling with the congruent preparation of technique, the thickness of single crystal super alloy testing piece subtract altogether
25 μm few, under this condition, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 24 μ m-thicks.
Embodiment 14
A kind of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 13, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 23 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 21.5 μ m-thicks.
Other modes are identical.
Embodiment 15
A kind of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 13, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 22 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 21 μ m-thicks.
Other modes are identical.
Embodiment 16
A kind of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 13.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 13, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 22 μm altogether, and under this condition, DD6 essence casting blade surface is divided out
In addition to 21 μ m-thicks.
Other modes are identical.
Embodiment 17
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 18molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.6molL-1,
MnO2Mass concentration is 3.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 18molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 0.6molL-1, MnO2Content is 3.0g
L-1Aqueous solution and ethyl orthosilicate by volume 1:3 prepare, revolution be 30 turns/min room temperature under be stirred 1h formed cream；
(2) milling etching time 180min；
It is 0.03~0.075%, Cr for C be 6.5~7.3%, Co be 7~8%, W is that 4.75~5.25%, Mo is
L.3~1.7%, Ta is that 6.5~6.7%, A1 is 5.8~6.4%, Y < 0.03%, and surplus is the nickel-base high-temperature single crystal alloy of Ni
Precision castings and single crystal super alloy testing piece milling with the congruent preparation of technique, the thickness of single crystal super alloy testing piece subtract altogether
19 μm few, under this condition, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 18 μ m-thicks.
Embodiment 18
A kind of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 17, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 19 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 19 μ m-thicks.
Other modes are identical.
Embodiment 19
A kind of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 17, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 19 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 18 μ m-thicks.
Other modes are identical.
Embodiment 20
A kind of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 17.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 17, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 19 μm altogether, and under this condition, DD6 essence casting blade surface is divided out
In addition to 18.5 μ m-thicks.
Other modes are identical.
Embodiment 21
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 18molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 2.0molL-1,
MnO2Mass concentration is 10.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 30 turns/min
Under revolving speed, 1h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 18molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 2.0molL-1, MnO2Content is 10g
L-1Aqueous solution and ethyl orthosilicate by volume 1:3 prepare, revolution be 30 turns/min room temperature under be stirred 2h formed cream；
(2) milling corrosion temperature is 30 ± 1 DEG C, etching time 90min；
(3) in ultrasonic cleaning, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, is containing nano-alpha aluminium oxide particle
Aqueous solution in, nano-alpha aluminium oxide particle partial size is 50nm, and the mass concentration of alpha aluminium oxide particle is 0.1gL-1, aqueous solution
Temperature is room temperature, pH value of water solution 7.
(4) supersonic frequency is 80kHz, time 30min；
It is 0.03~0.075%, Cr for C be 6.5~7.3%, Co be 7~8%, W is that 4.75~5.25%, Mo is
L.3~1.7%, Ta is that 6.5~6.7%, A1 is 5.8~6.4%, Y < 0.03%, and surplus is the nickel-base high-temperature single crystal alloy of Ni
Precision castings and single crystal super alloy testing piece milling with the congruent preparation of technique, the thickness of single crystal super alloy testing piece subtract altogether
20 μm few, under this condition, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 19 μ m-thicks.
Embodiment 22
A kind of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 21, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 12 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 11.3 μ m-thicks.
Other modes are identical.
Embodiment 23
A kind of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 21, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 15 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 14.6 μ m-thicks.
Other modes are identical.
Embodiment 24
A kind of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 21.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 21, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 9 μm altogether, and under this condition, DD5 essence casting blade surface about removes
8.2 μ m-thicks.
Other modes are identical.
Embodiment 25
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and ethyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and ethyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: ethyl orthosilicate=1:3；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 18molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 2.0molL-1,
MnO2Mass concentration is 10.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, ethyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 60 turns/min
Under revolving speed, 2h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 18molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 2.0molL-1, MnO2Content is
10.0g·L-1Aqueous solution and ethyl orthosilicate by volume 1:3 prepare, revolution be 60 turns/min room temperature under be stirred 2h
Form cream；
(2) milling corrosion temperature is 60 ± 1 DEG C, etching time 200min；
(3) in ultrasonic cleaning, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, is containing nano-alpha aluminium oxide particle
Aqueous solution in, nano-alpha aluminium oxide particle partial size is 300nm, and the mass concentration of alpha aluminium oxide particle is 2.0gL-1, water-soluble
Liquid temperature is room temperature, pH value of water solution 7.
(4) supersonic frequency is 10kHz, time 90min；
It is 0.03~0.075%, Cr for C be 6.5~7.3%, Co be 7~8%, W is that 4.75~5.25%, Mo is
L.3~1.7%, Ta is that 6.5~6.7%, A1 is 5.8~6.4%, Y < 0.03%, and surplus is the nickel-base high-temperature single crystal alloy of Ni
Precision castings and single crystal super alloy testing piece milling with the congruent preparation of technique, the thickness of single crystal super alloy testing piece subtract altogether
15 μm few, under this condition, nickel-base high-temperature single crystal alloy precision castings surface about eliminates 4 μ m-thicks, is unsatisfactory for application request,
It repeats step (2) and (3), the thickness of single crystal super alloy testing piece reduces by 10 μm, under this condition, nickel-based monocrystal altogether after tested
High temperature alloy precision castings surface about eliminates 9 μ m-thicks, meets application request.
Embodiment 26
A kind of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 25, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 10 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 9.3 μ m-thicks.
Other modes are identical.
Embodiment 27
A kind of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 25, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 12 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 11.6 μ m-thicks.
Other modes are identical.
Embodiment 28
A kind of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 25.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 25, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 13 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 12.2 μ m-thicks.
Other modes are identical.
Embodiment 29
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water and methyl orthosilicate；Wherein,
It is the mixing of mixed aqueous solution and methyl orthosilicate in single crystal super alloy precision castings milling cream, by volume, mixes water-soluble
Liquid: methyl orthosilicate=1:5；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 16molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 1.8molL-1,
MnO2Mass concentration is 6.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, methyl orthosilicate is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, in the stirring of 60 turns/min
Under revolving speed, 2h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 16molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 1.8molL-1, MnO2Content is 6.0g
L-1Aqueous solution and methyl orthosilicate 1:5 is prepared by volume, be stirred 1.5h in the case where revolution is 50 turns/min room temperature and formed
Cream；
(2) milling corrosion temperature is 60 ± 1 DEG C, etching time 200min；
(3) in ultrasonic cleaning, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, is containing nano-alpha aluminium oxide particle
Aqueous solution in, nano-alpha aluminium oxide particle partial size is 300nm, and the mass concentration of alpha aluminium oxide particle is 2.0gL-1, water-soluble
Liquid temperature is room temperature, pH value of water solution 7.
(4) supersonic frequency is 10kHz, time 90min；
(2) thickness of single crystal super alloy testing piece reduces 5 μm altogether, under this condition, nickel-base high-temperature single crystal alloy essence casting
Part surface about eliminates 4 μ m-thicks.
Other modes are identical.
Embodiment 30
A kind of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 29, difference is:
(1) single crystal super alloy precision castings are the DD32 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 14 μm altogether, and under this condition, DD32 essence casting blade surface is divided out
In addition to 13.1 μ m-thicks.
Other modes are identical.
Embodiment 31
A kind of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 29, difference is:
(1) single crystal super alloy precision castings are the DD5 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 13 μm altogether, and under this condition, DD5 essence casting blade surface is divided out
In addition to 12.6 μ m-thicks.
Other modes are identical.
Embodiment 32
A kind of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 29.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings local surfaces carry out milling, and chemical milling method, with embodiment 29, difference is:
(1) single crystal super alloy precision castings are the DD6 essence casting blade of as cast condition and the monocrystalline high temperature with the congruent preparation of technique
Alloy testing piece；
(2) thickness of single crystal super alloy testing piece reduces 8 μm altogether, and under this condition, DD5 essence casting blade surface about removes
7.6 μ m-thicks.
Other modes are identical.
Embodiment 33
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water, positive silicic acid propyl ester and positive silicic acid
Ethyl ester；Wherein, in single crystal super alloy precision castings milling cream, be mixed aqueous solution, positive silicic acid propyl ester, ethyl orthosilicate it is mixed
It closes, by volume, mixed aqueous solution: ethyl orthosilicate: positive silicic acid propyl ester=1:2:2；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 10molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 1.5molL-1,
MnO2Mass concentration is 5.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, comprising the following steps:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, the concentrated sulfuric acid is added to the water stirring, then sequentially adds FeCl3And MnO2, it stirs evenly,
Obtain sulfuric acid, FeCl3And MnO2Aqueous solution；
Step 2: mixing
According to the ratio, positive silicic acid propyl ester, ethyl orthosilicate are weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, 45
Turn/speed of agitator of min under, 2h is stirred at room temperature, single crystal super alloy precision castings milling cream is made.
A kind of application of single crystal super alloy precision castings milling cream is changed to carry out milling to single crystal super alloy precision castings
Milling method, with embodiment 1, difference is:
(1) it is 10molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 1.5molL-1, MnO2Content is 5.0g
L-1Aqueous solution and positive silicic acid propyl ester, ethyl orthosilicate mixture by volume 1:2:2 prepare, revolution be 45 turns/min it is normal
It is stirred 2h under temperature and forms cream；
(2) milling corrosion temperature is 50 ± 1 DEG C, etching time 120min；
(3) in ultrasonic cleaning, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, is containing nano-alpha aluminium oxide particle
Aqueous solution in, nano-alpha aluminium oxide particle partial size is 200nm, and the mass concentration of alpha aluminium oxide particle is 1.0gL-1, water-soluble
Liquid temperature is room temperature, pH value of water solution 7.
(4) supersonic frequency is 80kHz, time 30min；
(2) thickness of single crystal super alloy testing piece reduces 11.8 μm altogether, under this condition, nickel-base high-temperature single crystal alloy essence
Cast(ing) surface about eliminates 10.5 μ m-thicks.
Other modes are identical.
Embodiment 34
A kind of single crystal super alloy precision castings milling cream, including sulfuric acid, FeCl3、MnO2, water, positive silicic acid propyl ester and positive silicic acid
Ethyl ester；Wherein, in single crystal super alloy precision castings milling cream, be mixed aqueous solution, positive silicic acid propyl ester, ethyl orthosilicate it is mixed
It closes, by volume, mixed aqueous solution: butyl silicate=1:2；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 10molL that the content for each ingredient having, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 1.5molL-1,
MnO2Mass concentration is 5.0gL-1, surplus is water.
A kind of preparation method of single crystal super alloy precision castings milling cream, with embodiment 33.
A kind of application of single crystal super alloy precision castings milling cream is single crystal super alloy precision castings milling cream to monocrystalline height
Temperature alloy precision castings carry out milling, and chemical milling method, with embodiment 1, difference is:
(1) it is 10molL that milling cream, which is sulfuric acid concentration,-1, FeCl3Concentration is 1.5molL-1, MnO2Content is 5.0g
L-1Aqueous solution and butyl silicate by volume 1:2 prepare, revolution be 45 turns/min room temperature under be stirred 2h formed cream；
(2) overall surface is carried out to single crystal super alloy precision castings and carries out milling, the milling time is 180min.
(3) in ultrasonic cleaning, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle, is containing nano-alpha aluminium oxide particle
Aqueous solution in, nano-alpha aluminium oxide particle partial size is 50nm, and the mass concentration of alpha aluminium oxide particle is 2.0gL-1, aqueous solution
Temperature is room temperature, pH value of water solution 7.
(4) supersonic frequency is 50kHz, time 60min；
(2) thickness of single crystal super alloy testing piece reduces 19.2 μm altogether, under this condition, nickel-base high-temperature single crystal alloy essence
Cast(ing) surface about eliminates 18.7 μ m-thicks.
Other modes are identical.
Claims (10)
1. a kind of single crystal super alloy precision castings milling cream, which is characterized in that the single crystal super alloy precision castings milling cream includes
Sulfuric acid, FeCl3、MnO2, water and positive compound of silicate class；It wherein, is mixing water in single crystal super alloy precision castings milling cream
The mixing of solution and positive compound of silicate class, by volume, mixed aqueous solution: positive compound of silicate class=1:(2 ~ 5)；
Wherein, mixed aqueous solution is sulfuric acid, FeCl3And MnO2Aqueous solution, sulfuric acid, FeCl3And MnO2Aqueous solution in contain
It is 9 ~ 18molL that the content of each ingredient, which is respectively as follows: sulfuric acid molar concentration,-1, FeCl3Molar concentration is 0.3 ~ 2.0molL-1,
MnO2Mass concentration is 3.0 ~ 10.0gL-1, surplus is water.
2. single crystal super alloy precision castings milling cream as described in claim 1, which is characterized in that the positive silicate class
Conjunction object is the mixing of one or more of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate.
3. the preparation method of single crystal super alloy precision castings milling cream of any of claims 1 or 2, which is characterized in that including with
Lower step:
Step 1: matching Sulphuric acid, FeCl3And MnO2Aqueous solution
According to the ratio, raw material is weighed, by sulfuric acid, FeCl3And MnO2Mixing, stirs evenly, obtains sulfuric acid, FeCl3And MnO2It is water-soluble
Liquid；
Step 2: mixing
According to the ratio, positive compound of silicate class is weighed, with sulfuric acid, FeCl3And MnO2Aqueous solution mixing, 1 ~ 2h is stirred at room temperature, make
Obtain single crystal super alloy precision castings milling cream.
4. the preparation method of single crystal super alloy precision castings milling cream as claimed in claim 3, which is characterized in that the step
In rapid 2, the stirring, stirring rate is 30 ~ 60 turns/min.
5. the application of single crystal super alloy precision castings milling cream of any of claims 1 or 2, for single crystal super alloy precision castings
Carry out milling, which is characterized in that sequentially include the following steps:
(1) prepare
Handle single crystal super alloy precision castings: the surface impurity of cleaning single crystal super alloy precision castings obtains pretreated list
Brilliant high temperature alloy precision castings；
It prepares milling cream: according to the ratio, weighing raw material, prepare single crystal super alloy precision castings milling cream；
(2) milling cream is applied to the local surfaces and thickness of pretreated single crystal super alloy precision castings residual stress concentrations
In known testing piece, make the uniform smearing thickness 2- of testing piece known to pretreated single crystal super alloy precision castings and thickness
Painting is wiped testing piece known to the single crystal super alloy precision castings and thickness of milling cream and is heated to 30 ~ 60 DEG C by 3mm milling cream,
Corrode 90 ~ 200min, the testing piece after single crystal super alloy precision castings and corrosion after being corroded；
(3) by after the milling cream erasing on the single crystal super alloy precision castings after corrosion and the testing piece surface after corrosion, surpassed
Sonication cleaning, removal residual corrosion product, then be rinsed with water, it dries, according to the thickness change of testing piece, determines monocrystalline height
The removal amount of temperature alloy precision castings；
(4) when removal amount is unsatisfactory for application request or cannot completely remove surface plastic deformation layer, then repeatedly step (2) and
(3), until reaching application request.
6. the application of single crystal super alloy precision castings milling cream as claimed in claim 5, which is characterized in that the step
(1) in, the single crystal super alloy precision castings are nickel-base high-temperature single crystal alloy precision castings.
7. the application of single crystal super alloy precision castings milling cream as claimed in claim 6, which is characterized in that the Ni-based list
In brilliant high temperature alloy precision castings, the mass percent of the ingredient and each ingredient that contain is that C is 0.03% ~ 0.075%, Cr 6.5%
~ 7.3%, Co be 7% ~ 8%, W be 4.75% ~ 5.25%, Mo be l.3% ~ 1.7%, Ta be 6.5% ~ 6.7%, A1 be 5.8% ~ 6.4%, Y <
0.03%, surplus Ni.
8. the application of single crystal super alloy precision castings milling cream as claimed in claim 5, which is characterized in that the step
(2) in, the testing piece is the single crystal super alloy testing piece prepared using identical preparation process and same alloy ingredient.
9. the application of single crystal super alloy precision castings milling cream as claimed in claim 5, which is characterized in that the step
(3) in, in cleaned by ultrasonic vibration, cleaning solution is the aqueous solution containing nano-alpha aluminium oxide particle；
In aqueous solution containing nano-alpha aluminium oxide particle, nano-alpha aluminium oxide particle partial size is 50 ~ 300nm, alpha aluminium oxide particle
Mass concentration be 0.1 ~ 2.0gL-1, aqueous temperature is room temperature, and pH value of water solution is 7 ± 0.1.
10. the application of single crystal super alloy precision castings milling cream as claimed in claim 5, which is characterized in that the step
(3) in, for the ultrasonic frequency in 10 ~ 80kHz, the step (3), the ultrasonic cleaning time is 30 ~ 90min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4910834A (en) * | 1972-06-01 | 1974-01-30 | ||
| EP0049207B1 (en) * | 1980-10-01 | 1984-09-12 | United Technologies Corporation | Process for machining the surface of a nickel base superalloy workpiece |
| CN102817034A (en) * | 2012-08-24 | 2012-12-12 | 沈阳黎明航空发动机(集团)有限责任公司 | Chemical milling technology for surface plasticity deformation layer of single crystal cast blade |
| CN103451656A (en) * | 2013-08-31 | 2013-12-18 | 南昌航空大学 | Chemical milling method of K423A cast superalloy without intergranular corrosion |
| CN104923727A (en) * | 2015-05-15 | 2015-09-23 | 中国航空工业集团公司北京航空材料研究院 | Sand mould casting method of titanium or titanium alloy cast with special-shape inner hole |
| CN105483704A (en) * | 2015-11-23 | 2016-04-13 | 沈阳黎明航空发动机(集团)有限责任公司 | Deep chemical milling method of TA12 and TA15 titanium-alloy large-scale structural components |
-
2018
- 2018-04-19 CN CN201810352161.5A patent/CN108385108B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4910834A (en) * | 1972-06-01 | 1974-01-30 | ||
| EP0049207B1 (en) * | 1980-10-01 | 1984-09-12 | United Technologies Corporation | Process for machining the surface of a nickel base superalloy workpiece |
| CN102817034A (en) * | 2012-08-24 | 2012-12-12 | 沈阳黎明航空发动机(集团)有限责任公司 | Chemical milling technology for surface plasticity deformation layer of single crystal cast blade |
| CN103451656A (en) * | 2013-08-31 | 2013-12-18 | 南昌航空大学 | Chemical milling method of K423A cast superalloy without intergranular corrosion |
| CN104923727A (en) * | 2015-05-15 | 2015-09-23 | 中国航空工业集团公司北京航空材料研究院 | Sand mould casting method of titanium or titanium alloy cast with special-shape inner hole |
| CN105483704A (en) * | 2015-11-23 | 2016-04-13 | 沈阳黎明航空发动机(集团)有限责任公司 | Deep chemical milling method of TA12 and TA15 titanium-alloy large-scale structural components |
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