CN104451731B - Surface oxide layer chemical pickling liquid and application are removed containing Cr and Al elements high temperature alloy - Google Patents
Surface oxide layer chemical pickling liquid and application are removed containing Cr and Al elements high temperature alloy Download PDFInfo
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- CN104451731B CN104451731B CN201410709388.2A CN201410709388A CN104451731B CN 104451731 B CN104451731 B CN 104451731B CN 201410709388 A CN201410709388 A CN 201410709388A CN 104451731 B CN104451731 B CN 104451731B
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- oxide layer
- pickle
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
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- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The present invention relates to a kind of chemical pickling liquid containing Cr and Al elements high temperature alloy removal surface oxide layer and application, belong to the technology field that high temperature alloy chemistry method removes removing oxide layer.The composition of the pickle is:300~400g/L hydrochloric acid, 400~450g/L nitric acid and 100~150g/L hydrogen peroxide, remaining is water.For the high temperature alloy workpiece containing Cr and Al elements in Ni-based, iron-based and cobalt-based, surface oxide layer is removed using the synergy of the hydrochloric acid of certain concentration, nitric acid and hydrogen peroxide, each composition mechanism of action is as follows:Reactant is acted on high-temperature alloy surface oxide based on hydrochloric acid and nitric acid, and hydrogen peroxide accelerates the generation of reaction as catalyst.Substantially, efficiency high, the high-temperature alloy surface after treatment is bright, uniform for pickling effect of the present invention;Pickle of the present invention heat release during proportioning is low, safe without inflammable, sensitization and explosive reactant generation.
Description
Technical field
The present invention relates to a kind of chemical pickling liquid containing Cr and Al elements high temperature alloy removal surface oxide layer and application, category
The technology field of removing oxide layer is gone in high temperature alloy chemistry method.
Background technology
In Ni-based, iron-based and cobalt base superalloy, in order to improve the anti-oxidant and corrosion resistance of alloy, often closing
A certain amount of Cr elements are added in gold, the Cr good, fine and close to form adhesiveness2O3Type oxide-film.Meanwhile, the solid solution of alloy and heavy
Shallow lake intensified element Ni, Al etc. can also form NiO, Al2O3Oxide-film.Complicated alloying element causes that high temperature alloy oxide-film has
The characteristics of multilayer, complex phase, outer layer is with Cr2O3Based on, internal layer is with Al2O3Based on.Although this cause the anti-oxidant of high temperature alloy part and
Corrosion resistance is greatly improved, but also to hot forming and heat treatment after, weldment weldering before etc. go removing oxide layer to bring difficulty.Mesh
Before, the main removing oxide layer method of going for using has:Embrane method and chemical method are removed in mechanic shot peening method, craft.Although mechanic shot peening method energy
Removing oxide layer quickly is removed, but the roughness of alloy surface can be greatly improved simultaneously.For the workpiece with complex profile, because of it
It is high to shot-blast process parameter request and substantially reduce its oxide layer removal effect.And using embrane method is gone by hand, be then difficult to
Homogenization, the precision of workpiece can also therefore suffer from influence.At present, what industry use was more is chemical method, the pickling for being used
Liquid component is:Nitric acid+hydrofluoric acid+water or nitric acid+hydrofluoric acid+sulfuric acid+water etc..Chinese invention patent application (publication number
CN103934304A) mention, using nitric acid+hydrofluoric acid+water in mass ratio 0.5:2:7.5 pickles being mixed to get are closed to high temperature
Gold treatment.Chinese invention patent application (publication number CN103590057A) is proposed using nitric acid (190g/L-280g/L)+hydrofluoric acid
(10g/L-45g/L)+hydrochloric acid (10g/L-45g/L)+hexamethylenetetramine (1g/L-4g/L)+water, in 20 DEG C of -70 DEG C of pickling, place
The reason time was at -10 hours 2.5 hours.
In sum, in acid cleaning process, determine that treatment conditions include temperature and time, general effect according to pickling effect
Rate is relatively low, relatively costly.Such as when pickle is prepared especially with sulfuric acid, there is highly exothermic danger, use six first
Urotropine increases inflammable, sensitization and reactant has volatile danger.
The content of the invention
It is an object of the invention to provide a kind of chemical pickling that surface oxide layer is removed containing Cr and Al elements high temperature alloy
Liquid and application, can efficient, inexpensive, low dangerous removal high-temperature alloy surface oxide layer.
The technical scheme is that:
One kind removes surface oxide layer chemical pickling liquid containing Cr and Al elements high temperature alloy, and the composition of the pickle is:300
~400g/L hydrochloric acid, 400~450g/L nitric acid and 100~150g/L hydrogen peroxide, remaining is water.
Described remove surface oxide layer chemical pickling liquid containing Cr and Al elements high temperature alloy, pickle is preferably constituted
For:350g/L hydrochloric acid, 410g/L nitric acid and 130g/L hydrogen peroxide, remaining is water.
The described application that surface oxide layer chemical pickling liquid is removed containing Cr and Al elements high temperature alloy, specific steps are such as
Under:
(1) pretreatment of workpiece
It is cleaned by ultrasonic the oil stain and other pollutants of workpiece surface with alcohol or acetone;
(2) pickle is prepared
Using 300~400g/L of concentration hydrochloric acid, 400~450g/L nitric acid and 100~150g/L hydrogen peroxide, remaining is
Water, is poured into clean container successively, and pickle minimum volume meets can be completely immersed in workpiece;
(3) control of temperature
To fill in the container immersion thermostat of pickle, thermostat is using water, mixture of ice and water or liquid nitrogen refrigerating agent circulation
Cooled down, it is ensured that pickle temperature in acid cleaning process is less than 30 DEG C, it is to avoid vigorous reaction;
(4) acid cleaning process
Under conditions of the change of monitoring pickle temperature at any time, using plastic clamp clamping workpiece, it is put into pickle
Continuous vibration washing;
(5) cleaning of workpiece
After pickling terminates, it is cleaned by ultrasonic during workpiece quickly is moved into the container equipped with alcohol or acetone, is washed complete drying
.
The described application that surface oxide layer chemical pickling liquid is removed containing Cr and Al elements high temperature alloy, in conditions permit
In the case of, process workpiece surface using plastic bruss.
The described application that surface oxide layer chemical pickling liquid is removed containing Cr and Al elements high temperature alloy, container immersion is logical to follow
In the thermostat of ring water cooling, it is ensured that pickle temperature in acid cleaning process is preferably 5 DEG C~20 DEG C, vibrated in pickle clear
Wash 5~30 minutes.
Advantages of the present invention and beneficial effect are:
1st, substantially, efficiency high, the high-temperature alloy surface after treatment is bright, uniform for pickling effect of the present invention;
2nd, pickle of the present invention heat release during proportioning is low, without inflammable, sensitization and explosive reactant generation, security
It is high.
3rd, present invention high temperature alloy workpiece containing Cr and Al elements suitable for Ni-based, iron-based and cobalt-based.
Brief description of the drawings
Fig. 1 is using the test piece schematic diagram after pickling of the present invention.
Specific embodiment
For the high temperature alloy workpiece containing Cr and Al elements in Ni-based, iron-based and cobalt-based, using the hydrochloric acid of certain concentration, nitre
The synergy removal surface oxide layer of acid and hydrogen peroxide, each composition mechanism of action is as follows:It is anti-based on hydrochloric acid and nitric acid
Ying Tiyu high-temperature alloy surfaces oxide is acted on, and hydrogen peroxide accelerates the generation of reaction as catalyst.
The use process of chemical pickling liquid of the present invention containing Cr and Al elements high temperature alloy removal surface oxide layer is as follows:
(1) pretreatment of workpiece
It is cleaned by ultrasonic the oil stain and other pollutants of workpiece surface with alcohol or acetone.
(2) pickle is prepared
Using 300~400g/L of concentration hydrochloric acid, 400~450g/L nitric acid and 100~150g/L hydrogen peroxide, remaining is
Water, pours into clean container successively, as long as pickle minimum volume meets can be completely immersed in workpiece.
(3) control of temperature
To fill in the container immersion thermostat of pickle, thermostat is followed using refrigerants such as water, mixture of ice and water or liquid nitrogen
Ring is cooled down, it is ensured that pickle temperature in acid cleaning process is less than 30 DEG C, it is to avoid vigorous reaction.
(4) acid cleaning process
Under conditions of the change of monitoring pickle temperature at any time, using plastic clamp clamping workpiece, it is put into pickle
Continuous vibration washing;Workpiece surface can be processed using plastic bruss in the case of conditions permit, accelerate acid cleaning process, further carried
Pickling efficiency high.
(5) cleaning of workpiece
After pickling terminates, it is cleaned by ultrasonic during workpiece quickly is moved into the container equipped with alcohol or acetone, is washed complete drying
.
Below by embodiment and accompanying drawing, the present invention is described in more detail.
Embodiment
As shown in figure 1, the heat treatment strips of nickel base superalloy IN 718 have oxide layer, the present embodiment is to nickel-base high-temperature
Alloy IN 718 is heat-treated the pickling of test piece.
Using plastic clamp, the alloy test pieces of IN 718 after solid solution at 980 DEG C 10 hours are directly placed into dress pickle
Pickling is carried out in container.Pickle is constituted:Concentration 350g/L hydrochloric acid, 410g/L nitric acid and 130g/L hydrogen peroxide, remaining is
Water.In the thermostat of the logical circulating water of container immersion, it is ensured that pickle temperature in acid cleaning process is less than 30 DEG C (generally 5
DEG C~20 DEG C), vibration washing 10 minutes in pickle.After end, it is 99wt% ethanol quickly to move to equipped with concentration test piece
Carry out being cleaned by ultrasonic 3 minutes in solution, wash and finish drying.
As shown in figure 1, compared with original blank, strip oxide layer is removed completely after pickling, and surface-brightening is uniform.
Embodiment result shows, with pickle component in the prior art:" 1. nitric acid+hydrofluoric acid+water, 2. nitric acid+hydrofluoric acid
+ sulfuric acid+water, 3. nitric acid+hydrofluoric acid+hydrochloric acid+hexamethylenetetramine+water " is compared, using the hydrochloric acid of certain concentration of the present invention, nitre
Acid and hydrogen peroxide, hydrogen peroxide accelerate the generation of reaction as catalyst, and its technical characterstic and benefit are:
1st, pickling reaction speed of the present invention is fast, efficiency high;
2nd, substantially, the high-temperature alloy surface after treatment is bright, uniform for pickling effect of the present invention;
3rd, acid cleaning process temperature of the present invention is relatively low and controllable, and working environment is friendly;
4th, pickle of the present invention heat release during proportioning is low, without inflammable, sensitization and explosive reactant generation, security
It is high.
Claims (1)
1. a kind of application that surface oxide layer chemical pickling liquid is removed containing Cr and Al elements high temperature alloy, it is characterised in that specific
Step is as follows:
The heat treatment strips of nickel base superalloy IN 718 have oxide layer, to the heat treatment test pieces of nickel base superalloy IN 718
Pickling;
Using plastic clamp, the alloy test pieces of IN 718 after solid solution at 980 DEG C 10 hours are directly placed into the container of dress pickle
In carry out pickling;Pickle is constituted:Concentration 350g/L hydrochloric acid, 410g/L nitric acid and 130g/L hydrogen peroxide, remaining is water;Hold
In the thermostat of the logical circulating water of device immersion, it is ensured that pickle temperature in acid cleaning process is 5 DEG C~20 DEG C, in pickle
Vibration washing 10 minutes;After end, test piece is moved to equipped with concentration to carry out being cleaned by ultrasonic 3 minutes in 99wt% ethanol solutions, washed
Finish drying;Strip oxide layer is removed completely after pickling, and surface-brightening is uniform.
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CN108411315A (en) * | 2018-04-17 | 2018-08-17 | 贵州振华群英电器有限公司(国营第八九厂) | A kind of cleaning technology of TO-5 cases outside and the fifth wheel of inner cavity |
CN110670078A (en) * | 2019-10-30 | 2020-01-10 | 攀钢集团江油长城特殊钢有限公司 | Acid pickling method for eliminating GH4099 alloy along crystal oxide layer |
CN111139488A (en) * | 2020-03-03 | 2020-05-12 | 广东富行洗涤剂科技有限公司 | Chemical demolding liquid for high-temperature alloy and demolding treatment method thereof |
CN112665952B (en) * | 2020-10-29 | 2023-03-24 | 北京星航机电装备有限公司 | GH3128 high-temperature alloy welding seam metallographic structure corrosive agent and corrosion method |
CN112962104B (en) * | 2021-02-02 | 2022-12-23 | 乐普(北京)医疗器械股份有限公司 | Method for removing laser processing slag on metal surface and application |
CN115261862A (en) * | 2022-09-06 | 2022-11-01 | 清华大学 | Corrosive agent for corroding nickel-based single crystal superalloy, corrosion method and device for realizing method |
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CN102443794B (en) * | 2011-12-06 | 2013-07-24 | 中国科学院金属研究所 | Aluminum alloy scratch resistant and fingerprint resistant chromium-free chemical conversion solution for ship and preparation method of conversion film |
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