CN105603500B - Magnesium alloy residual stress detects the electrolytic polishing liquid and electrolytic polishing method of pre-treatment - Google Patents
Magnesium alloy residual stress detects the electrolytic polishing liquid and electrolytic polishing method of pre-treatment Download PDFInfo
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- CN105603500B CN105603500B CN201610021357.7A CN201610021357A CN105603500B CN 105603500 B CN105603500 B CN 105603500B CN 201610021357 A CN201610021357 A CN 201610021357A CN 105603500 B CN105603500 B CN 105603500B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/18—Polishing of light metals
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Abstract
The present invention provides electrolytic polishing liquids and electrolytic polishing method that a kind of magnesium alloy residual stress detects pre-treatment；Electrolytic polishing liquid of the present invention includes that volume ratio is 1:1‑2:23 phosphoric acid, glycerine and absolute ethyl alcohol.The electrolytic polishing liquid of the present invention, be conducive to obtain accurate residual stress testing result, using this kind of electrolytic polishing liquid polishing process, easy to operate, polishing effect is stablized simultaneously, compared with existing product, has the advantages that raw material sources are extensive, it is simple, of low cost to prepare；The invention also discloses it is a kind of easy to operate, it can be achieved that magnesium alloy successively polishing, processing speed is fast and the electrobrightening for the detection pre-treatment of magnesium alloy residual stress of effect stability sends out method.
Description
Technical field
The present invention relates to technical field of magnesium alloy surface treatment, specifically, before being related to a kind of detection of magnesium alloy residual stress
The electrolytic polishing liquid and electrolytic polishing method of processing.
Background technology
Magnesium alloy is that have high specific strength, specific stiffness and good magnetic cup than lightest structural metallic materials at present
The advantages that covering property, damping and amortization, and rich reserves, are 2.3% in the resource content of veneer of crust metallic ore, occupy common metal
4th, be a kind of structural material in the fields such as automobile and aerospace with broad prospect of application.Particularly, a large amount of to use
Magnesium alloy manufacture aerospace equipment parts by be the following aerospace career development important directions, can reach maximum subtract
Weight effect.But, this type component has higher requirement to fatigue behaviour, wide in production to further increase its fatigue strength
It is general to use the surface intensified techniques such as shot-peening, rolling, purposefully residual compressive stress is introduced in material surface.
The importance that quantitatively characterizing is material and Mechanical Engineering Development is carried out to residual stress.Currently without direct
Method can accurate measurement remnant stress intensity.There are four types of the methods of typical measurement remnant stress：X-ray diffraction method；In
Sub- diffraction approach；Boring method；Indentation method.The most commonly used is X-ray diffraction methods at present.The base of X-ray diffraction measurement residualinternal stress
Present principles are to measure diffracted ray displacement as initial data, measured result is practical according to Bragg equation 2dsin θ=n λ
On be overstrain, and residual stress is calculated by Hooke's law by overstrain.But, X-ray penetrates depth
Degree is smaller, can only measure the residual stress of material surface, if necessary to measure the residual stress of material internal, or measures stress
Gradient needs to use layer stripping.Sample is successively removed, measures the stress per layer surface.Therefore, measurement remnant stress it
Before, it needs to carry out electrobrightening to sample.In addition, magnesium alloy is similar to the residual stress of steel and aluminum generation rule, but
Magnesium alloy has the crystal structure of close-packed hexagonal, and anisotropy is also easy to produce in process, therefore, is applied to the conjunctions such as steel and aluminium
The electrolytic polishing liquid of gold is not suitable for magnesium alloy.
The magnesium alloy residual stress detection pre-treatment electrolytic polishing liquid that the present country uses is the AC-2 business of external import
Polishing fluid, 5000 yuan/liter of price, now the product foreign countries stop production comprehensively, the country without similar products production, sell.Currently, state
Interior researcher mainly uses the method for oneself preparing electrolytic polishing liquid to carry out the processing before residual stress detection to magnesium alloy, but
Many places are in the exploratory stage, and since the ingredient of Related product is uncertain, ratio is uncertain, therefore effect is unstable.
Existing patent CN201010566667 provides a kind of electrolytic polishing liquid for magnesium alloy texture detection pre-treatment
And electrolytic polishing process, but its successively polishing efficiency is not high.
Invention content
For the defects in the prior art, an object of the present invention is to provide a kind of preceding place of magnesium alloy residual stress detection
The electrolytic polishing liquid of reason, the electrolytic polishing liquid derive from a wealth of sources, prepare texture calibration rate height after simple, of low cost and polishing；This
There is provided the electrolytic polishing method that a kind of magnesium alloy residual stress detects pre-treatment, this method synthesis to make for the second purpose of invention
With mechanical agitation and magnetic agitation can Rapid Cleaning fall the magnesium alloy that specimen surface dissolved, successively polishing efficiency is high.
The present invention is achieved by the following technical solutions：
The present invention provides a kind of electrolytic polishing liquid of magnesium alloy residual stress detection pre-treatment, and the electrolytic polishing liquid includes
Following components：Phosphoric acid, glycerine and absolute ethyl alcohol；The volume ratio of the phosphoric acid, glycerine and absolute ethyl alcohol is 1:1-2:2-3.Wherein
The effect of phosphoric acid is Mg alloy surface to be dissolved in polishing process, and form phosphate coating on surface, prevents magnesium alloy table
Face excessive erosion, glycerine can dissolve each other with water arbitrary proportion, and phosphoric acid can be assisted to form mucous membrane in Mg alloy surface, to reach control
The purpose of corrosion rate, absolute ethyl alcohol then can suitably reduce the viscosity of solution, increase the electric conductivity of solution.However phosphoric acid is glutinous
Spend larger, the phosphate of generation also has prodigious viscosity.Glycerol content is too low, and magnesium alloy dissolving is too fast, causes rough surface
It spends larger, is unfavorable for the measurement of follow-up residual stress；Too high levels, then polishing fluid viscosity increase, operation difficulty increase.Anhydrous second
The addition of alcohol then plays the role of that viscosity is made to reduce, and improves electric conductivity, and operation is made to be easy to carry out.In summary factor consideration and reality
It tests as a result, the volume ratio of phosphoric acid, glycerine and absolute ethyl alcohol is 1:1-2:2-3 is most appropriate.
Preferably, the volume ratio of the phosphoric acid, glycerine and absolute ethyl alcohol is 1:1:2.
The present invention also provides the electrolytic polishing methods that a kind of magnesium alloy residual stress detects pre-treatment, including following step
Suddenly：
1) using magnesium alloy sample as anode, it is connected with constant current regulated power supply anode, and immerses and fill electrobrightening above-mentioned
In the electrolytic vessel of liquid；
2) using stainless steel substrates as cathode, and it is connected with constant current regulated power supply cathode, in the step 1) electrolytic polishing liquid
Carry out electrobrightening to get.
Preferably, in step 2), the electrobrightening time is 4~8min, and polishing voltage is 2~6V；Polishing electric current is
0.8~1.2A.
It is highly preferred that the electrobrightening time is 5min, polishing voltage is 4V, and polishing electric current is 1A.
Preferably, further include being passed through liquid nitrogen into cell vessel before electrobrightening electrolysis is made to throw in the step 2)
The step of light liquid temperature is down to subzero 10 DEG C to subzero 30 DEG C.The reason of selecting the temperature range be primarily due to temperature less than-
30 DEG C, texture calibration rate is less than 75%, and temperature is higher than -10 DEG C, and texture calibration rate is less than 82%.
Preferably, in step 2), the electrobrightening carries out under agitation.
It is highly preferred that the stirring is to be stirred using magnetic stirring apparatus and mechanical agitator.Synthesis is stirred using machinery
Mix and stir magnetic agitation can Rapid Cleaning fall the magnesium alloy that specimen surface has dissolved, successively polishing efficiency is high.
During electrobrightening, the magnesium in magnesium alloy sample loses electronics, promote magnesium anode occur cell reaction and it is molten
Solution, as electrolysis time increases, electrolyte layers are continuously increased, and specimen surface is in silver bright color.Wherein electrolysis time cannot be long, if
Electrolysis time is long, and one side specimen surface forms oxidation film, is on the other hand unfavorable for obtaining the stationary value of residual stress.
Compared with prior art, the present invention has following advantageous effect：
1. the electrolytic polishing liquid of the present invention is conducive to obtain accurate residual stress testing result, while this kind electrolysis is thrown
Light liquid polishing process is easy to operate, and polishing effect is stablized；
2. the present invention electrolytic polishing liquid compared with existing product, have raw material sources extensively, prepare it is simple, of low cost
The advantages of；
3. the electrolytic polishing process of the present invention it is easy to operate, it can be achieved that magnesium alloy successively polishing, processing speed is fast and imitates
Fruit is stablized.
Other advantages, target and the feature of the present invention will be illustrated in the following description to a certain extent, and
To a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, or can be with
It is instructed from the practice of the present invention.The target and other advantages of the present invention can pass through following description and claims
Book is realized and is obtained.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is electrolytic polishing method operation chart；
Wherein：1- phosphoric acid, glycerine, absolute ethyl alcohol mixed liquor；2- heater switch；3- magnetic stirring apparatus；4- magnetic beads；5- temperature
Degree meter；6- anodes；7- crossing current regulated power supplies；8- cathodes；9- blenders；10- liquid nitrogen；11- power switches.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
The electrolytic polishing method operation chart that the present invention uses is as shown in Figure 1, include：1- phosphoric acid, glycerine, anhydrous second
Alcohol mixed liquor；2- heater switch；3- magnetic stirring apparatus；4- magnetic beads；5- thermometers；6- anodes；7- crossing current regulated power supplies；8- is cloudy
Pole；9- blenders；10- liquid nitrogen；11- power switches.
Embodiment 1
In the present embodiment, use phosphoric acid, glycerine, absolute ethyl alcohol volume ratio for 1:1:2 mixed solution is ZK60 to the trade mark
The magnesium alloy after shot-peening rolls handled, electrolytic polishing method operation is as shown in Figure 1.The magnesium alloy is a kind of typical
Magnesium alloy materials, test result are of universal significance.Specific electrolytic polishing method is as shown in Figure 1, include the following steps：
1) using magnesium alloy sample as anode, and it is connected with constant current regulated power supply anode and immerses the electricity for filling electrolytic polishing liquid
Solve container in, the electrolytic polishing liquid be phosphoric acid, glycerine, absolute ethyl alcohol volume ratio be 1:1:2 mixed solution；
2) using stainless steel substrates as cathode, and it is connected with constant current regulated power supply cathode, electricity is carried out in aforementioned electrolytic polishing liquid
Solution polishes, and it is subzero 10 DEG C to subzero 30 DEG C to be passed through liquid nitrogen before electrobrightening into cell vessel and keep solution temperature.Electrolysis
Polishing time is 5min, and polishing voltage is 4v, and polishing electric current is 1A.
The operating voltage range of the constant current regulated power supply is 0-50V, ranging from 0.1~3A of voltage is operated, polished
Cheng Zhong, the magnesium in magnesium alloy sample lose electronics, promote magnesium anode that cell reaction occurs and dissolves, as electrolysis time increases,
Electrolyte layers are continuously increased, and specimen surface is in silver bright color.Wherein electrolysis time cannot be long, if electrolysis time is long, on the one hand
Specimen surface forms oxidation film, is on the other hand unfavorable for obtaining the stationary value of residual stress.After polishing for the first time, surveyed with X-ray
Stress value at this time is obtained, second is carried out and polishes, then measure the stress value after second of delamination.And so on, until measuring
Data are more stable, obtain a stationary value.In addition, this sample is carried out residual stress test with synchrotron radiation, comparison is stablized
Value and synchrotron radiation measured value.It is 92% to measure the ratio between the stationary value and synchrotron radiation measured value in embodiment 1.Illustrate embodiment
The residual-stress value of gained it is accurate and reliable.In addition, its texture calibration rate is 90%, illustrate that embodiment is reliable residual in acquisition
Higher texture rate can also be obtained except residue stress value.
Embodiment 2~9
ZK60 magnesium alloys after being rolled to same shot-peening by using different concentration and processing parameter (as shown in table 1)
It is handled.
Table 1
From above example as can be seen that voltage, electric current, electrolysis time selection in a small range for residual stress
The influence of measurement result is little, but the ratio of phosphoric acid, glycerine, absolute ethyl alcohol on sample residual stress analysis result influence compared with
Greatly, with phosphoric acid, glycerine, absolute ethyl alcohol volume ratio for 1:1:2 mixed solution is as electrolytic polishing liquid, polishing time 4-8min
Sample residual stress, the ratio of the measured value of X-ray and the measured value of synchrotron radiation should be used as most 90% or more
Good solution concentration and polishing time use.In addition, use individually magnetic agitation in polishing process uses machine with comprehensive
Tool stirring, magnetic agitation are made comparisons, the results showed that and it is comprehensive to use mechanical agitation and magnetic agitation, it can realize and successively throw faster
Light, reason mainly in polishing process, comprehensive stirring can Rapid Cleaning fall the magnesium alloy that specimen surface has dissolved, to
Improve successively polishing efficiency.
Comparative example 1-2
Electrolytic polishing liquid uses the nitric acid wine of the preferred electrolytic polishing liquids of patent CN201010566667, that is, a concentration of 35%
ZK60 magnesium alloys after essence rolls same shot-peening are handled, as a result as follows：
Comparative example 3
This comparative example is identical as 1 method of embodiment, differs only in：The electrolytic polishing liquid is phosphoric acid, absolute ethyl alcohol
Volume ratio is 1:2 mixed solution.Thus the X-ray measurement value of ZK60 magnesium alloys that treated and the ratio of synchrotron radiation measured value
Value is 80%, and texture calibration rate is 75%, is below 1 measured value of embodiment, shows that glycerine is added in polishing fluid to be conducive to obtain
Preferable experimental result.
By comparison, it can be found that electrolytic polishing liquid and polishing process that the present embodiment is invented preferably can be used to survey
Determine the residual stress of magnesium alloy.
In conclusion the electrolytic polishing liquid of the present invention, is conducive to obtain accurate residual stress testing result, while this kind
Electrolytic polishing liquid polishing process is easy to operate, and polishing effect is stablized；The electrolytic polishing liquid of the present invention compared with existing product, has
Raw material sources are extensive, prepare advantage simple, of low cost；The electrolytic polishing process of the present invention is easy to operate, it can be achieved that magnesium closes
The successively polishing of gold, processing speed is fast and effect stability.
Specific embodiments of the present invention and comparative example are described above.Except the range cited by embodiment, at this
Other respective ranges of invention protection can equally be implemented.It is to be appreciated that the invention is not limited in above-mentioned specific
Embodiment, those skilled in the art can make various deformations or amendments within the scope of the claims, this has no effect on this
The substantive content of invention.
Claims (8)
1. a kind of electrolytic polishing liquid of magnesium alloy residual stress detection pre-treatment, which is characterized in that the electrolytic polishing liquid by with
The following group is grouped as：Phosphoric acid, glycerine and absolute ethyl alcohol；The volume ratio of the phosphoric acid, glycerine and absolute ethyl alcohol is 1:1-2:2-3；Institute
It is ZK60 to state magnesium alloy.
2. the electrolytic polishing liquid of magnesium alloy residual stress detection pre-treatment according to claim 1, which is characterized in that described
The volume ratio of phosphoric acid, glycerine and absolute ethyl alcohol is 1:1:2.
3. a kind of electrolytic polishing method of magnesium alloy residual stress detection pre-treatment, which is characterized in that include the following steps：
1) using magnesium alloy sample as anode, it is connected with constant current regulated power supply anode, and immerses and fill electrolysis described in claim 1
In the electrolytic vessel of polishing fluid；
2) using stainless steel substrates as cathode, and it is connected with constant current regulated power supply cathode, is carried out in the step 1) electrolytic polishing liquid
Electrobrightening to get.
4. the electrolytic polishing method of magnesium alloy residual stress detection pre-treatment according to claim 3, which is characterized in that step
It is rapid 2) in, time of the electrobrightening is 4~8min, and polishing voltage is 2~6V；Polishing electric current is 0.8~1.2A.
5. the electrolytic polishing method of magnesium alloy residual stress detection pre-treatment according to claim 4, which is characterized in that institute
It is 5min to state the electrobrightening time, and polishing voltage is 4V, and polishing electric current is 1A.
6. the electrolytic polishing method of magnesium alloy residual stress detection pre-treatment according to claim 3, which is characterized in that institute
It states in step 2), further includes being passed through liquid nitrogen into cell vessel before electrobrightening electrolytic polishing liquid temperature is made to be down to subzero 10
DEG C to subzero 30 DEG C the step of.
7. the electrolytic polishing method of magnesium alloy residual stress detection pre-treatment according to claim 3, which is characterized in that step
It is rapid 2) in, the electrobrightening carries out under agitation.
8. the electrolytic polishing method of magnesium alloy residual stress detection pre-treatment according to claim 7, which is characterized in that institute
It is specially to be stirred using magnetic stirring apparatus and mechanical agitator to state stirring.
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| CN110804751B (en) * | 2019-10-14 | 2022-03-08 | 平高集团有限公司 | Pretreatment method for preparing metal coating on surface of cast metal piece, cast metal piece metal coating part and preparation method thereof |
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| CN101829364B (en) * | 2010-06-22 | 2013-07-17 | 上海交通大学 | Method for preparing biodegradable magnesium alloy intravascular stent |
| CN101985772B (en) * | 2010-12-01 | 2012-10-03 | 重庆大学 | Electrolytic polishing solution and electrolytic polishing process for detection pretreatment of magnesium alloy texture |
| CN102140671B (en) * | 2011-04-07 | 2013-05-01 | 上海交通大学 | Electrochemical polishing method of degradable magnesium alloy endovascular stent |
| CN102337580A (en) * | 2011-09-21 | 2012-02-01 | 合肥金盟工贸有限公司 | Ion liquid polishing solution for electrochemically polishing magnesium alloy and preparation method thereof |
| CN103938262A (en) * | 2013-01-23 | 2014-07-23 | 汉达精密电子(昆山)有限公司 | Magnesium alloy electrochemical polishing solution and method of processing magnesium alloy with the polishing solution |
| CN104073868B (en) * | 2014-06-18 | 2016-08-31 | 郑州大学 | A kind of electrochemical process for treating being applicable to magnesium alloy intervention apparatus and auxiliary equipment |
| CN105154963A (en) * | 2015-08-17 | 2015-12-16 | 奚廷斐 | Electrolytic polishing solution for magnesium alloy medical heart stent and surface polishing processing technology of medical heart stent |
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