CN114018793B - Coating for reducing impact sensitivity of titanium alloy gas cylinder and coating evaluation method - Google Patents
Coating for reducing impact sensitivity of titanium alloy gas cylinder and coating evaluation method Download PDFInfo
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- CN114018793B CN114018793B CN202111274862.XA CN202111274862A CN114018793B CN 114018793 B CN114018793 B CN 114018793B CN 202111274862 A CN202111274862 A CN 202111274862A CN 114018793 B CN114018793 B CN 114018793B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 117
- 238000000576 coating method Methods 0.000 title claims abstract description 117
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 52
- 230000035945 sensitivity Effects 0.000 title claims abstract description 24
- 238000011156 evaluation Methods 0.000 title abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 179
- 239000007789 gas Substances 0.000 claims abstract description 109
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000007747 plating Methods 0.000 claims abstract description 56
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000010949 copper Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000002791 soaking Methods 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 23
- 239000001301 oxygen Substances 0.000 claims description 23
- 229910052760 oxygen Inorganic materials 0.000 claims description 23
- 230000008859 change Effects 0.000 claims description 13
- 238000009863 impact test Methods 0.000 claims description 12
- 238000011010 flushing procedure Methods 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 6
- 238000009991 scouring Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims 2
- 238000003860 storage Methods 0.000 abstract description 7
- 238000013461 design Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a plating layer for reducing impact sensitivity of a titanium alloy gas cylinder, which comprises a nickel preplating layer, a copper preplating layer and a copper acid plating layer which are plated on the outer surface of the titanium alloy gas cylinder in sequence, wherein the impact sensitivity of the titanium alloy gas cylinder in a liquid oxygen environment is reduced through the design of the thickness of each layer, and the safe use of the titanium alloy gas cylinder in the liquid oxygen environment is ensured; the invention also discloses a method for evaluating the coating, which designs a test piece test and a bottle test for evaluating the coating according to the use condition, and enables the test condition to be more similar to the real use condition through the tests of liquid oxygen circulation soaking, liquid oxygen mechanical impact, repeated temperature circulation, repeated inflation and the like, thereby realizing the effective evaluation of the reliability of the coating in the liquid oxygen environment and having wide application prospect in the storage field of pressurized gas.
Description
Technical Field
The invention belongs to the field of preparation and evaluation of titanium alloy gas cylinders, and relates to a coating for reducing mechanical impact sensitivity of a titanium alloy gas cylinder in a liquid oxygen environment and an evaluation method.
Background
The carrier rocket pressurizing and conveying system usually adopts a normal-temperature high-pressure gas cylinder to pressurize the storage tank, so that the inlet pressure of the rocket engine and the rigidity of the storage tank are ensured to meet the use requirement of flying. With the development of space technology, the requirement of a launching task on rocket carrying capacity is greatly improved, and the pressurization scheme of the normal-temperature high-pressure gas cylinder is difficult to meet the use requirement. The high-temperature high-pressure gas cylinder pressurizing scheme (engineering is called cold helium pressurizing) can improve the storage density of pressurizing gas and the structure efficiency of pressurizing the gas cylinder, and the cold helium pressurizing is applied to a plurality of models at home and abroad at present. The existing cold helium pressurization scheme mostly adopts a titanium alloy metal gas cylinder as a storage container, and simultaneously places the gas cylinder in a hydrogen tank, and uses liquid hydrogen as a cold source to cool the pressurized gas in the gas cylinder, so that the effect of storing the pressurized gas in high density is achieved, and the pressurization efficiency and carrying capacity are greatly improved.
Although the cold helium pressurization technology is mature, it is mostly applied to models or modules with liquid hydrogen environment at present. For the type using liquid oxygen and kerosene propellant, there is also a need for storing pressurized gas at high density, but in view of the fact that available cold source is low-temperature liquid oxygen, the compatibility of titanium alloy materials with liquid oxygen is a key problem. Because of the many factors affecting the stability of titanium alloys under liquid oxygen, there is currently no international recognition that limits the application of the cold helium pressurization scheme.
Disclosure of Invention
The invention aims to overcome the defects and provide a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder, which comprises a nickel preplating layer, a copper preplating layer and a copper acid plating layer which are plated on the outer surface of the titanium alloy gas cylinder in sequence, wherein the impact sensitivity of the titanium alloy gas cylinder in a liquid oxygen environment is reduced through the design of the thickness of each layer, and the safe use of the titanium alloy gas cylinder in the liquid oxygen environment is ensured; the invention also provides a method for evaluating the coating, which designs a test piece test and a bottle test for evaluating the coating according to the use condition, enables the test condition to be more similar to the real use condition through the tests of liquid oxygen circulation soaking, liquid oxygen mechanical impact, repeated temperature circulation, repeated inflation and the like, realizes the effective evaluation of the reliability of the coating in the liquid oxygen environment, and has wide application prospect in the storage field of pressurized gas
In order to achieve the above purpose, the present invention provides the following technical solutions:
the plating layer for reducing the impact sensitivity of the titanium alloy gas cylinder comprises a nickel preplating layer, a copper preplating layer and a copper acid plating layer which are plated on the outer surface of the titanium alloy gas cylinder in sequence;
the total thickness of the nickel preplating layer, the copper preplating layer and the acid copper plating layer is d, the thickness of the nickel preplating layer is 60-75 percent d, the thickness of the copper preplating layer is 15-25 percent d, the thickness of the acid copper plating layer is 5-20 percent d, and the sum of the thicknesses of the nickel preplating layer, the copper preplating layer and the acid copper plating layer is 100 percent d.
Further, the thickness of the nickel preplating layer is 60% d, the thickness of the copper preplating layer is 25% d, and the thickness of the acid copper plating layer is 15% d.
A method for evaluating a coating, wherein the coating is evaluated to be reliable in a liquid oxygen environment when the coating passes a test piece test and a whole bottle test simultaneously;
the test piece test comprises a liquid oxygen circulation soaking test, a liquid oxygen and gas oxygen scouring test and a liquid oxygen mechanical impact test; the bottle test comprises repeated temperature cycle test and repeated inflation test;
the specific method for the liquid oxygen cycle soaking test comprises the following steps:
(1.1) placing the titanium alloy coating test piece in liquid oxygen for soaking, taking out and recovering to room temperature;
(1.2) after repeating the step (1.1) for 5-8 times, evaluating that the coating passes the liquid oxygen cycle soaking test if the appearance of the test piece has no obvious change;
the specific method for the liquid oxygen and gas oxygen scouring test comprises the following steps: the titanium alloy coating test pieces are alternately flushed with 0.5MPa liquid oxygen and gas oxygen for 5-10 min respectively, the flushing times are equal to or more than 1 time for each liquid oxygen and gas oxygen, the preferable scheme is that each liquid oxygen and gas oxygen are flushed for 1 time, and the coating is evaluated to pass the liquid oxygen and gas oxygen flushing test if the appearance of the test pieces does not change obviously;
the specific method for the liquid oxygen mechanical impact test comprises the following steps: in a liquid oxygen environment, a punch is adopted to impact a titanium alloy coating test piece with 98J energy, and the condition that the coating passes the liquid oxygen mechanical impact test is that more than or equal to 20 test pieces have no flash or more than or equal to 60 test pieces have less flash than 1;
the specific method for repeated temperature cycle test comprises the following steps:
(2.1) soaking the titanium alloy coating gas cylinder in liquid oxygen, taking out and recovering to room temperature;
(2.2) after the gas cylinder is used for more than or equal to 2 to 5 times of the number of times in the repeated step (2.1), evaluating that the coating passes the repeated temperature cycle test if the appearance of the coating has no obvious change;
the specific method for the repeated inflation test comprises the following steps:
(3.1) inflating the titanium alloy coating gas cylinder to a pressure which is more than or equal to 1-2 times of the gas cylinder using pressure, and maintaining the pressure for 1-3 min and then deflating;
and (3.2) repeating the step (3.1) for more than or equal to 2 to 5 times of the use times of the gas cylinder, and evaluating that the coating passes the repeated inflation test if the appearance of the coating has no obvious change.
Further, in the evaluation method of the coating, the titanium alloy coating used in the test piece test is in a round plate shape, the diameter of the test piece is 10 mm-15 mm, and the thickness of the coating of the test piece is calculated according to the following formula:
wherein delta 1 For the thickness of the coating of the test piece, delta 2 The thickness of the gas cylinder coating is R is the radius of the gas cylinder when the gas cylinder is not inflated, and delta R is the variation of the radius of the gas cylinder after the gas cylinder is inflated to the use pressure relative to R.
Further, in the method for evaluating the coating, in the step (1.1) of the liquid oxygen cycle soaking test, the test piece coated with the coating is placed in the liquid oxygen for soaking for 48-72 hours, and then is taken out and is freely restored to the room temperature.
Furthermore, in the assessment method of the coating, in the step (1.2) of the liquid oxygen cycle soaking test and in the liquid oxygen and gas oxygen flushing test, the standard that the appearance of the test piece has no obvious change is that a 10-time magnifying glass is adopted to observe the surface of the test piece, oxidation spots do not appear on the surface of the test piece, and cracks do not appear on the surface of the coating.
Further, in the method for evaluating a plating layer, in the repeated temperature cycle test step (2.1), the gas cylinder is taken out and freely returned to room temperature.
Further, in the method for evaluating the coating, in the step (2.2) of the repeated temperature cycle test, the number of times of repeated step (2.1) is equal to 4 times of the number of times of use of the gas cylinder, and the coating is evaluated to pass the repeated temperature cycle test without obvious change of the appearance of the coating;
in the step (3.1) of repeated inflation test, inflating the gas cylinder plated with the coating to the pressure equal to 1.5 times of the gas cylinder use pressure, and maintaining the pressure for 1min and then deflating;
in the step (3.2), the number of times of repeating the step (3.1) is equal to 4 times of the number of times of using the gas cylinder, and the coating is evaluated to pass the repeated inflation test if the appearance of the coating is not obviously changed.
Furthermore, in the method for evaluating the coating, in the step (2.2) of repeated temperature cycle test and the step (3.2) of repeated inflation test, the standard that the appearance of the coating has no obvious change is that a 10-time magnifying glass is adopted to observe the surface of the coating, and the surface of the coating does not crack or fall off.
Further, in the assessment method of the coating, the coating is used for reducing the impact sensitivity of the liquid oxygen environment of the titanium alloy gas cylinder.
Compared with the prior art, the invention has the following beneficial effects:
(1) The coating for reducing the impact sensitivity of the titanium alloy gas cylinder in the liquid oxygen environment is designed, the composition and thickness of each layer of the coating of the gas cylinder are designed, the mechanical impact sensitivity of the titanium alloy gas cylinder in the liquid oxygen environment can be reduced, the coating is prevented from cracking and falling off after repeated temperature cycle, inflation and other tests, and the gas cylinder in the whole life cycle is ensured to be used safely and reliably;
(2) The invention creatively provides a method for evaluating the coating, which comprehensively considers the use condition of the gas cylinder, evaluates the reliability of the coating in a liquid oxygen environment from two layers of a test piece and the whole gas cylinder, provides specific evaluation standards and has wide application prospect in the field of storage of pressurized gas;
(3) In the assessment method of the coating, the test piece is designed according to the deformation working condition of the actual gas cylinder, so that the accuracy of assessment is effectively improved.
Drawings
FIG. 1 is a schematic illustration of a coating for reducing the impact sensitivity of a titanium alloy cylinder in a liquid oxygen environment according to the present invention.
Detailed Description
The features and advantages of the present invention will become more apparent and clear from the following detailed description of the invention.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. Although various aspects of the embodiments are illustrated in the accompanying drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The conventional titanium alloy metal gas cylinder has a spherical structure, as shown in fig. 1, wherein 1 is a metal cylinder body, 2 is a filler neck connected with an external pipeline, 3 is a plug, 4 is a metal plating layer prepared by the invention, 41 is a nickel preplating layer, 42 is a copper preplating layer, and 43 is a copper acid plating layer. In the metal coating prepared by the invention, the bonding capability of the coating and the outer surface of the gas cylinder is enhanced by adopting a nickel preplating method, and the copper coating is completed by adopting two copper plating processes of preplating copper and acid plating copper.
The plating layer arrangement of the invention not only considers the technical feasibility, but also needs to consider the structural integrity of the plating layer under the working condition of repeated inflation and deflation, thereby avoiding the local falling of the plating layer after inflation for several times and affecting the safe use. Therefore, the strength and the hardness of the coating are gradually increased from inside to outside, the inner layer adopts soft materials (nickel preplating layers) to strengthen the fluidity, the outer layer adopts hard materials (copper acid plating layers) to strengthen the structural stability, and the coating does not fall off in the repeated use process. Proved by calculation and test, the thickness of the nickel preplating layer material is more than 60% of the whole plating layer, the thickness of the copper preplating layer material is 20% of the whole plating layer, the thickness of the outer copper plating layer (copper acid plating layer) accounts for about 15% of the whole plating layer thickness, and the anti-repeated inflation fatigue effect is optimal.
The effect of the titanium alloy gas cylinder coating on reducing the mechanical impact sensitivity in the liquid oxygen environment is verified through a test piece test and a whole cylinder test. The titanium alloy coating test piece and the whole bottle can ensure safe use under the liquid oxygen environment after passing the following test. The titanium alloy coating test piece material is in a round piece shape, the thickness of the coating in the test piece preparation process can not be directly determined according to the thickness of the coating, the thickness setting is carried out according to the deformation working condition of an actual gas cylinder, and otherwise, the sufficiency of the test is affected. The calculation can be specifically performed with reference to the following formula:
wherein delta 1 For the thickness of the coating of the test piece, delta 2 The thickness of the gas cylinder coating is R is the radius of the gas cylinder when the gas cylinder is not inflated, and delta R is the variation of the radius of the gas cylinder after the gas cylinder is inflated to the use pressure relative to R.
The test piece test and the whole bottle test comprise the following specific steps:
1) Test piece test:
1.1 Liquid oxygen circulation soaking: the liquid oxygen is soaked for 48 hours and then returns to room temperature, the repeated circulation is carried out for 5 times, after the liquid oxygen soaking of 1 round is completed, the next round of soaking test is carried out after the liquid oxygen soaking of 1 round is thoroughly restored to room temperature, the structural materials and the coating are ensured to be fully deformed, and after the test is finished, the appearance of a test piece is not obviously changed, and the coating is assessed to pass the liquid oxygen circulating soaking test;
after the test is finished, the appearance of the test piece has no obvious change, namely, after the test is finished, a 10-time magnifying glass is adopted to observe the surface of the test piece, oxidation spots do not appear on the surface, and cracks do not appear on the surface of a coating.
1.2 Liquid oxygen/gas oxygen flushing): the liquid oxygen and the gas oxygen of 0.5MPa are adopted to alternately wash, the washing time is 5-10 min respectively, the appearance is not obviously changed after the test is finished, the coating is assessed to pass the liquid oxygen/gas oxygen washing test, and the appearance of the test piece is not obviously changed after the test is finished, the coating is assessed to pass the liquid oxygen/gas oxygen washing test;
1.3 Liquid oxygen mechanical impact test): in a liquid oxygen environment, a punch is adopted to impact the test piece with 98J energy, 20 test pieces have no flash or 60 test pieces have less flash than 1 test piece, and the plating layer is evaluated to pass the liquid oxygen mechanical impact test.
2) Whole bottle test:
2.1 Repeated warm-cycling test): repeatedly soaking at low temperature and naturally returning to the temperature (soaking at the low temperature in liquid oxygen of 80K-100K and naturally returning to the temperature of more than 293K), and evaluating that the coating passes the repeated temperature cycle test if the coating does not crack or fall off;
2.2 Repeated inflation test): repeatedly inflating and deflating, and evaluating the coating through repeated inflating tests if the coating does not crack or fall off, wherein the inflating pressure in the test is determined according to the using conditions, the inflating and deflating cycle times are determined according to the using times of the gas cylinder, and in a preferred scheme, the inflating pressure is equal to 1.5 times of the using pressure of the gas cylinder, and the inflating and deflating cycle times are equal to 4 times of the using times of the gas cylinder.
Example 1:
in the embodiment, a plating layer for reducing impact sensitivity of a titanium alloy gas cylinder in a liquid oxygen environment is prepared by adopting the following method:
the thickness of the nickel preplating layer material is determined to be 60% of the total thickness of the plating layer, the thickness of the copper preplating layer material is determined to be 25% of the total thickness of the plating layer, and the thickness of the outer layer of acid copper plating layer is 15% of the longitudinal thickness of the plating layer. The total thickness of the plating layer is 10-15 mu m.
The preparation process of the plating layer comprises the following steps:
pre-plating treatment: comprises the steps of deoiling (organic deoiling, electrolytic deoiling), cleaning (water-purifying flushing, deionized water cleaning), activating treatment, acid cleaning, mixed acid cleaning and the like. And carrying out subsequent plating processing after finishing the plating pretreatment.
Nickel pre-plating: nickel plating is carried out by adopting an electroplating nickel method, the processing thickness delta (t) is controlled by controlling the processing time t, the thickness is measured by adopting an ultrasonic method after the processing is finished, the requirement of the thickness proportion is met, and deionized water is adopted for cleaning.
Copper preplating and acid copper plating: copper plating is carried out by adopting an electro-coppering method, the processing thickness delta (t) is controlled by controlling the processing time t, the thickness is measured by adopting an ultrasonic method after the processing is finished, the requirement of the thickness proportion is met, and deionized water is adopted for cleaning. And carrying out passivation treatment and drying to finish the coating of the plating layer.
In this embodiment, the evaluation of the plating layer includes test piece test and bottle test, and the specific method is as follows:
1) Test piece test:
1.1 Liquid oxygen circulation soaking: the liquid oxygen is soaked for 48 hours and then returns to room temperature, the repeated circulation is carried out for 5 times, after the liquid oxygen soaking of 1 round is completed, the next round of soaking test is carried out after the liquid oxygen soaking of 1 round is thoroughly restored to room temperature, the structural materials and the coating are ensured to be fully deformed, and after the test is finished, the appearance of a test piece is not obviously changed, and the coating is assessed to pass the liquid oxygen circulating soaking test;
after the test is finished, the appearance of the test piece has no obvious change, namely, after the test is finished, a 10-time magnifying glass is adopted to observe the surface of the test piece, oxidation spots do not appear on the surface, and cracks do not appear on the surface of a coating.
1.2 Liquid oxygen/gas oxygen flushing): the liquid oxygen and the gas oxygen of 0.5MPa are adopted to alternately wash, the washing time is 5-10 min respectively, the appearance is not obviously changed after the test is finished, the coating is assessed to pass the liquid oxygen/gas oxygen washing test, and the appearance of the test piece is not obviously changed after the test is finished, the coating is assessed to pass the liquid oxygen/gas oxygen washing test;
1.3 Liquid oxygen mechanical impact test): in a liquid oxygen environment, the test piece is impacted by a punch with 98J energy, 20 test pieces have no flash or 60 test pieces have less than 1 flash, and the test piece passes the liquid oxygen mechanical impact test.
2) Whole bottle test:
2.1 Repeated warm-cycling test): repeating the low-temperature soaking and natural temperature returning for 12 times (the low-temperature soaking is performed in liquid oxygen at 80K-100K and the natural temperature returning is performed to more than 293K), and evaluating that the coating passes the repeated temperature cycle test if the coating does not crack or fall off;
2.2 Repeated inflation test): and (3) repeatedly inflating and deflating for 12 times, and evaluating that the coating passes the repeated inflation test if the coating does not crack or fall off, wherein the inflation pressure in the test is determined according to the use condition.
Test piece test and whole bottle test results meet the requirements, and the coating can be reliably applied in a liquid oxygen environment.
In the embodiment, the prepared coating test piece test for reducing the impact sensitivity of the titanium alloy gas cylinder in the liquid oxygen environment and the whole cylinder test result meet the requirements, and the reliable application in the liquid oxygen environment can be satisfied; the titanium alloy test piece without a coating is adopted to perform 98J energy impact test pieces, the number of flashing pieces/test piece number is 3/20 and 5/60 respectively, microcracks appear on the surface of the titanium alloy test piece with a single copper coating after 5 times of temperature cycle, the 98J energy impact test piece is performed, and the number of flashing pieces/test piece number is 1/20 and 2/60 respectively, so that reliable application in a liquid oxygen environment cannot be satisfied.
The invention has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
What is not described in detail in the present specification is a well known technology to those skilled in the art.
Claims (9)
1. The plating layer for reducing the impact sensitivity of the titanium alloy gas cylinder is characterized by comprising a nickel preplating layer, a copper preplating layer and a copper acid plating layer which are plated on the outer surface of the titanium alloy gas cylinder in sequence;
the total thickness of the nickel preplating layer, the copper preplating layer and the acid copper plating layer is d, the thickness of the nickel preplating layer is 60-75 percent d, the thickness of the copper preplating layer is 15-25 percent d, and the thickness of the acid copper plating layer is 5-20 percent d;
the total thickness of the plating layer is 10-15 mu m.
2. The plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder according to claim 1, wherein the thickness of the nickel preplating layer is 60% d, the thickness of the copper preplating layer is 25% d, and the thickness of the acid copper plating layer is 15% d.
3. A method for evaluating a coating for reducing the impact sensitivity of a titanium alloy cylinder according to claim 1 or 2, wherein the coating is evaluated as being reliable in a liquid oxygen environment when passing both the test piece test and the whole cylinder test;
the test piece test comprises a liquid oxygen circulation soaking test, a liquid oxygen and gas oxygen scouring test and a liquid oxygen mechanical impact test; the bottle test comprises repeated temperature cycle test and repeated inflation test;
the specific method for the liquid oxygen cycle soaking test comprises the following steps:
(1.1) placing the titanium alloy coating test piece in liquid oxygen for soaking, taking out and recovering to room temperature;
(1.2) after repeating the step (1.1) for 5-8 times, evaluating that the coating passes the liquid oxygen cycle soaking test if the appearance of the test piece has no obvious change;
the specific method for the liquid oxygen and gas oxygen scouring test comprises the following steps: the titanium alloy coating test pieces are alternately flushed by liquid oxygen and gas oxygen for 5 to 10 minutes respectively, and the coating is assessed to pass the liquid oxygen and gas oxygen flushing test if the appearance of the test pieces is not obviously changed;
the specific method for the liquid oxygen mechanical impact test comprises the following steps: in a liquid oxygen environment, a punch is adopted to impact a titanium alloy coating test piece with 98J energy, and the condition that the coating passes a liquid oxygen mechanical impact test is that more than or equal to 20 test pieces have no flash;
the specific method for repeated temperature cycle test comprises the following steps:
(2.1) soaking the titanium alloy coating gas cylinder in liquid oxygen, taking out and recovering to room temperature;
(2.2) after the times of repeating the step (2.1) are more than or equal to 2 times of the times of using the gas cylinder, evaluating that the coating passes the repeated temperature cycle test if the appearance of the coating has no obvious change;
the specific method for the repeated inflation test comprises the following steps:
(3.1) inflating the titanium alloy coating gas cylinder to the use pressure of the gas cylinder with the pressure not less than 1 time, and maintaining the pressure for 1-3 min and then deflating;
and (3.2) repeating the step (3.1) for more than or equal to 2 times of the use times of the gas cylinder, and evaluating that the coating passes the repeated inflation test if the appearance of the coating has no obvious change.
4. A method for evaluating a plating layer for reducing impact sensitivity of a titanium alloy gas cylinder according to claim 3, wherein the titanium alloy plating layer used in the test of the test piece is in the form of a circular plate having a diameter of 10mm to 15mm, and the thickness of the plating layer of the test piece is calculated according to the following formula:
wherein delta 1 For the thickness of the coating of the test piece, delta 2 The thickness of the gas cylinder coating is R is the radius of the gas cylinder when the gas cylinder is not inflated, and delta R is the variation of the radius of the gas cylinder after the gas cylinder is inflated to the use pressure relative to R.
5. The method for evaluating a coating for reducing impact sensitivity of a titanium alloy gas cylinder according to claim 3, wherein in the step (1.1) of the liquid oxygen cycle immersion test, the test piece coated with the coating is immersed in liquid oxygen for 48 to 72 hours, and then taken out and freely restored to room temperature;
the specific method for the liquid oxygen and gas oxygen scouring test comprises the following steps: the test pieces of the titanium alloy coating are alternately flushed with liquid oxygen and gas oxygen at 0.5MPa for 5-10 min, and the coating is evaluated to pass the liquid oxygen and gas oxygen flushing test if the appearance of the test pieces is not changed obviously.
6. A method for evaluating a plating layer for reducing impact sensitivity of a titanium alloy gas cylinder according to claim 3, wherein in the step (1.2) of the liquid oxygen cycle immersion test and in the liquid oxygen and gas oxygen flushing test, the standard that the appearance of the test piece is not significantly changed is that the surface of the test piece is observed by using a 10-fold magnifying glass, no oxidized spots appear on the surface of the test piece and no cracks appear on the surface of the plating layer.
7. A method of evaluating a coating for reducing the impact sensitivity of a titanium alloy cylinder according to claim 3, wherein in the repeated warm-cycle test step (2.1), the cylinder is removed and allowed to return freely to room temperature.
8. The method for evaluating a plating layer for reducing impact sensitivity of a titanium alloy gas cylinder according to claim 3, wherein in the step (2.2) of repeating the temperature cycle test, the number of times of repeating the step (2.1) is equal to 4 times of the number of times of gas cylinder use, and the plating layer is evaluated to pass the repeating temperature cycle test without significant change in the appearance of the plating layer;
in the step (3.1) of repeated inflation test, inflating the gas cylinder plated with the coating to the pressure equal to 1.5 times of the gas cylinder use pressure, and maintaining the pressure for 1min and then deflating;
in the step (3.2), the number of times of repeating the step (3.1) is equal to 4 times of the number of times of using the gas cylinder, and the coating is evaluated to pass the repeated inflation test if the appearance of the coating is not obviously changed.
9. A method for evaluating a coating for reducing impact sensitivity of a titanium alloy gas cylinder according to claim 3, wherein in the repeated temperature cycle test step (2.2) and the repeated inflation test step (3.2), the coating appearance is not significantly changed by observing the surface of the coating with a 10-fold magnifying glass, and no cracks or falling off occur on the surface of the coating.
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