CN114018793A - 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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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 47
- 230000035945 sensitivity Effects 0.000 title claims abstract description 18
- 238000011156 evaluation Methods 0.000 title claims abstract description 17
- 239000011248 coating agent Substances 0.000 title claims description 74
- 238000000576 coating method Methods 0.000 title claims description 74
- 238000012360 testing method Methods 0.000 claims abstract description 179
- 239000007789 gas Substances 0.000 claims abstract description 106
- 238000007747 plating Methods 0.000 claims abstract description 103
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 88
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052802 copper Inorganic materials 0.000 claims abstract description 35
- 239000010949 copper Substances 0.000 claims abstract description 35
- 238000002791 soaking Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 239000010410 layer Substances 0.000 claims description 103
- 238000000034 method Methods 0.000 claims description 34
- 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 17
- 238000011010 flushing procedure Methods 0.000 claims description 15
- 238000007654 immersion Methods 0.000 claims description 11
- 238000009863 impact test Methods 0.000 claims description 11
- 238000009991 scouring Methods 0.000 claims description 7
- 239000011247 coating layer Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 6
- 238000012545 processing 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
- 239000007788 liquid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 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
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005259 measurement Methods 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
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical compound [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000005002 finish coating 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
- 238000000746 purification Methods 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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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Abstract
The invention discloses a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder, which comprises a pre-plated nickel layer, a pre-plated copper layer and a copper acid plating layer which are sequentially plated on the outer surface of the titanium alloy gas cylinder, 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 plating layer evaluation method, wherein a test piece test and a whole bottle test for evaluating the plating layer are designed according to the use working condition, and the test conditions are closer to the real use conditions through tests such as liquid oxygen cyclic soaking, liquid oxygen mechanical impact, repeated temperature cycle, repeated inflation and the like, so that the reliability of the plating layer in a liquid oxygen environment is effectively evaluated, and the plating layer evaluation method has a wide application prospect in the field of pressurized gas storage.
Description
Technical Field
The invention belongs to the field of preparation and evaluation of a titanium alloy gas cylinder, and relates to a coating for reducing the mechanical impact sensitivity of the titanium alloy gas cylinder in a liquid oxygen environment and an evaluation method.
Background
The carrier rocket pressurization 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 can meet the flight use requirements. Along with the development of space technology, the requirement of a launching task on the carrying capacity of a rocket is greatly improved, and the pressurization scheme of the normal-temperature high-pressure gas cylinder cannot meet the use requirement. The low-temperature high-pressure gas cylinder pressurization scheme (which is called cold helium pressurization in engineering) can improve the storage density of the pressurized gas and improve the structural efficiency of gas cylinder pressurization, and the cold helium pressurization 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 box, and cools the pressurized gas in the gas cylinder by taking liquid hydrogen as a cold source, so that the effect of storing the pressurized gas at high density is achieved, and the pressurization efficiency and the carrying capacity are greatly improved.
Although the helium cooling pressurization technology is mature, most of the technology is applied to models or modules with liquid hydrogen environment. For the model adopting liquid oxygen and kerosene propellant, the requirement of high-density storage of pressurized gas also exists, but in view of the fact that the available cold source is low-temperature liquid oxygen, the compatibility of the titanium alloy material and the liquid oxygen becomes a key problem. Because the factors influencing the stability of the titanium alloy under liquid oxygen are more, the current international recognition is not unified, and the application of a cold helium pressurizing scheme is limited.
Disclosure of Invention
The invention aims to overcome the defects and provides a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder, which comprises a pre-plated nickel layer, a pre-plated copper layer and a copper acid plating layer which are sequentially plated on the outer surface of the titanium alloy gas cylinder, 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, so that the safe use of the titanium alloy gas cylinder in the liquid oxygen environment is ensured; the invention also provides a plating layer evaluation method, which designs a test piece test and a whole bottle test for evaluating the plating layer according to the use working condition, and the test conditions are closer to the real use conditions through the tests of liquid oxygen cyclic soaking, liquid oxygen mechanical impact, repeated temperature cycle, repeated inflation and the like, thereby realizing the effective evaluation of the reliability of the plating layer in the liquid oxygen environment, and having wide application prospect in the field of pressurized gas storage
In order to achieve the above purpose, the invention provides the following technical scheme:
a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder comprises a pre-plated nickel layer, a pre-plated copper layer and an acid copper layer which are sequentially plated on the outer surface of the titanium alloy gas cylinder;
the total thickness of the pre-nickel plating layer, the pre-copper plating layer and the acid copper plating layer is recorded as d, the thickness of the pre-nickel plating layer is 60% -75% d, the thickness of the pre-copper plating layer is 15% -25% d, the thickness of the acid copper plating layer is 5% -20% d, and the sum of the thicknesses of the pre-nickel plating layer, the pre-copper plating layer and the acid copper plating layer is 100% d.
Furthermore, the thickness of the nickel pre-plating layer is 60% d, the thickness of the copper pre-plating layer is 25% d, and the thickness of the copper acid plating layer is 15% d.
When the plating layer passes a test piece test and a whole bottle test at the same time, the evaluation of the plating layer is reliable in a liquid oxygen environment;
the test piece test comprises a liquid oxygen cycle immersion test, a liquid oxygen and gas oxygen scouring test and a liquid oxygen mechanical impact test; the whole bottle test comprises a repeated temperature cycle test and a repeated inflation test;
the specific method of the liquid oxygen cycle immersion test comprises the following steps:
(1.1) soaking the titanium alloy coating test piece in liquid oxygen, taking out and recovering to room temperature;
(1.2) after repeating the step (1.1) for 5-8 times, evaluating that the plating layer passes a liquid oxygen cycle immersion test if the appearance of the test piece has no obvious change;
the specific method of the liquid oxygen and gas oxygen scouring test is as follows: alternately flushing the titanium alloy coating test piece with 0.5MPa of liquid oxygen and gas oxygen for 5-10 min respectively, wherein the flushing frequency is that the liquid oxygen and the gas oxygen are more than or equal to 1 time respectively, the preferred scheme is that the liquid oxygen and the gas oxygen are flushed for 1 time respectively, and the coating is evaluated to pass the liquid oxygen and gas oxygen flushing test if the appearance of the test piece is not obviously changed;
the specific method of 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 through a liquid oxygen mechanical impact test is that no flash exists in more than 20 test pieces or flash is less than 1 in more than 60 test pieces;
the specific method for repeating the 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 step (2.1) is repeated for more than or equal to 2-5 times of the using times of the gas cylinder, evaluating that the plating layer passes a repeated temperature cycle test if the appearance of the plating layer has no obvious change;
the specific method of the repeated inflation test comprises the following steps:
(3.1) inflating the gas cylinder with the titanium alloy coating until the pressure is more than or equal to 1-2 times of the using pressure of the gas cylinder, maintaining the pressure for 1-3 min, and then deflating;
and (3.2) repeating the step (3.1) for more than or equal to 2-5 times of the using times of the gas cylinder, and evaluating that the plating layer passes a repeated inflation test if the appearance of the plating layer does not obviously change.
Further, in the method for evaluating the coating, a test piece of the titanium alloy coating used in the test piece test is in a disc 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:
Further, in the method for evaluating the plating layer, in the step (1.1) of the liquid oxygen cycle immersion test, the test piece plated with the plating layer is placed in liquid oxygen for immersion for 48 to 72 hours, and then is taken out and is freely recovered to the room temperature.
Further, in the method for evaluating the plating layer, the step (1.2) of the liquid oxygen cycle immersion test and the liquid oxygen and gas oxygen scouring test have the standard that the test piece surface does not have obvious change by observing the test piece surface by using a magnifying lens with the magnification of 10 times, no oxidation spots appear on the test piece surface, and no cracks appear on the plating layer surface.
Further, in the evaluation method of the plating layer, in the repeated temperature cycle test step (2.1), the gas cylinder is taken out and freely returned to the room temperature.
Further, in the method for evaluating the plating layer, in the step (2.2) of the repeated temperature cycle test, the number of times of repeating the step (2.1) is equal to 4 times of the number of times of using the gas cylinder, and the plating layer is evaluated to pass the repeated temperature cycle test if the appearance of the plating layer is not obviously changed;
in the step (3.1) of the repeated inflation test, the gas cylinder plated with the plating layer is inflated until the pressure is equal to 1.5 times of the using pressure of the gas cylinder, and the gas is deflated after the pressure is maintained for 1 min;
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 plating layer is evaluated to pass a repeated inflation test if the appearance of the plating layer is not obviously changed.
Further, in the evaluation method of the coating, in the step (2.2) of the repeated temperature cycle test and the step (3.2) of the repeated inflation test, the standard that the appearance of the coating has no obvious change is that the coating surface is observed by a magnifying glass with the magnification of 10 times, and no crack or shedding occurs on the coating surface.
Further, in a method for evaluating the plating layer, the plating layer 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 plating layer for reducing the impact sensitivity of the titanium alloy gas cylinder in the liquid oxygen environment is designed, the composition and the thickness of each layer of the plating layer of the gas cylinder are designed, the mechanical impact sensitivity of the titanium alloy gas cylinder in the liquid oxygen environment can be reduced, and the plating layer does not crack or fall off after repeated temperature cycling, inflation and other tests, so that the gas cylinder in the whole life cycle is ensured to be used safely and reliably;
(2) the invention innovatively provides an evaluation method of a coating, which comprehensively considers the use working condition of a gas cylinder, evaluates the reliability of the coating in a liquid oxygen environment from two aspects of a test piece and the whole cylinder, and provides a specific evaluation standard;
(3) according to the evaluation method of the coating, the test piece is designed according to the deformation condition of the actual gas cylinder, and the evaluation accuracy is effectively improved.
Drawings
FIG. 1 is a schematic diagram of a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder to liquid oxygen environment according to the invention.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively 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. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The existing titanium alloy metal gas cylinder is of a spherical structure, as shown in fig. 1, 1 is a metal cylinder body, 2 is a filler neck connected with an external pipeline, 3 is a plug, and 4 is a metal plating layer prepared by the invention, wherein 41 is a pre-plated nickel layer, 42 is a pre-plated copper layer, and 43 is a plated copper layer. In the metal coating prepared by the invention, the bonding capacity of the coating and the outer surface of the gas cylinder is enhanced by adopting a nickel preplating method, and the copper coating is finished by adopting two copper plating processes of copper preplating and acid copper plating.
The coating is arranged by considering the feasibility of the process, and the structural integrity of the coating under the working condition of repeated inflation and deflation, so that the coating is prevented from locally falling off after being inflated for several times and influencing the safe use. Therefore, the strength and hardness of the selected materials of the plating layer are increased step by step from inside to outside, the inner layer adopts soft materials (pre-plated nickel layer) to enhance the fluidity, the outer layer adopts hard materials (plated copper acid layer) to enhance the structural stability, and the plating layer does not fall off in the repeated use process. Through calculation and test verification, the thickness of the nickel pre-plating layer material is more than 60% of the thickness of the whole plating layer, the thickness of the copper pre-plating layer material is 20% of the thickness of the whole plating layer, the thickness of the outer copper plating layer (acid copper plating layer) accounts for about 15% of the thickness of the whole plating layer, and the repeated inflation fatigue resistance 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 by a test piece test and a whole cylinder test. The titanium alloy coating test piece and the whole bottle can be used safely in liquid oxygen environment after the following tests. The titanium alloy coating test piece material is in a disc shape, the coating thickness can not be directly determined according to the coating thickness in the test piece preparation process, the thickness setting is carried out according to the actual gas cylinder deformation working condition, and otherwise, the test sufficiency is influenced. Specifically, the following formula can be referred to for calculation:
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 temperature is recovered to the room temperature after the liquid oxygen soaking for 48 hours, the cycle is repeated for 5 times, after 1 round of liquid oxygen soaking is finished, the room temperature is completely recovered, the next round of soaking test is carried out, the structural material and the coating are ensured to be fully deformed, and the coating is evaluated to pass the liquid oxygen cycle soaking test if the appearance of the test piece is not obviously changed after the test is finished;
the fact that the appearance of the test piece has no obvious change after the test is finished means that after the test is finished, the surface of the test piece is observed by a magnifying lens with the magnification of 10 times, oxidation spots do not appear on the surface, and cracks do not appear on the surface of a coating.
1.2) liquid/gas oxygen flush: flushing is carried out alternately by adopting liquid oxygen and gas oxygen under 0.5MPa, the flushing time is 5-10 min respectively, the appearance of the coating passes through the liquid oxygen/gas oxygen flushing test without obvious change after the test is finished, and the coating passes through the liquid oxygen/gas oxygen flushing test if the appearance of the test piece does not change obviously after the test is finished;
1.3) liquid oxygen mechanical impact test: and (3) under the liquid oxygen environment, a punch is adopted to impact the test piece with 98J energy, and the condition that 20 test pieces have no flash or 60 test pieces have less than 1 flash is judged that the coating passes the liquid oxygen mechanical impact test.
2) And (3) whole bottle test:
2.1) repeated temperature cycle test: repeatedly soaking at low temperature and naturally returning to the temperature (soaking at the low temperature in liquid oxygen of 80-100K, and naturally returning to the temperature of over 293K), and evaluating that the plating passes a repeated temperature cycle test if the plating does not crack or fall off;
2.2) repeated inflation test: and repeatedly inflating and deflating, wherein if the plating layer is not cracked or dropped, the plating layer is evaluated to pass a repeated inflation test, the inflation pressure in the test is determined according to the use working condition, and the inflation and deflation cycle times are determined according to the use time requirements of the gas cylinder, in a preferred scheme, the inflation pressure is equal to 1.5 times of the use pressure of the gas cylinder, and the inflation and deflation cycle times are equal to 4 times of the use times of the gas cylinder.
Example 1:
in the embodiment, a plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder in a liquid oxygen environment is prepared in the following manner:
the thickness of the material of the pre-plated nickel layer is determined to be 60% of the total thickness of the plating layer, the thickness of the material of the pre-plated copper layer is determined to be 25% of the total thickness of the plating layer, and the thickness of the acid copper plating layer of the outer layer accounts for 15% of the longitudinal thickness of the plating layer. The total thickness of the plating layer is 10 to 15 μm.
The preparation process of the coating comprises the following steps:
pre-plating treatment: the method comprises the steps of deoiling (organic deoiling and electrolytic deoiling), cleaning (water purification washing and deionized water cleaning), activating treatment, acid cleaning, mixed acid cleaning and the like of the gas cylinder. And performing subsequent plating processing after the plating pretreatment is finished.
Pre-nickel plating: and (3) nickel plating is carried out by adopting an electro-nickelling method, the processing thickness delta (t) is controlled by controlling the processing time t, the thickness measurement is carried out by adopting an ultrasonic method after the processing is finished, the requirement of the thickness proportion is ensured to be met, and deionized water is adopted for cleaning.
Pre-plating copper and acid copper: copper plating is carried out by adopting an electro-coppering method, the processing thickness delta (t) is controlled by controlling the processing time t, after the completion, the thickness measurement is carried out by adopting an ultrasonic method, the requirement of the thickness proportion is ensured to be met, and deionized water is adopted for cleaning. And carrying out passivation treatment and drying to finish coating of the coating.
In this embodiment, the evaluation of the plating layer, including a test piece test and a whole bottle test, is performed by the following specific method:
1) test piece test:
1.1) liquid oxygen circulation soaking: the temperature is recovered to the room temperature after the liquid oxygen soaking for 48 hours, the cycle is repeated for 5 times, after 1 round of liquid oxygen soaking is finished, the room temperature is completely recovered, the next round of soaking test is carried out, the structural material and the coating are ensured to be fully deformed, and the coating is evaluated to pass the liquid oxygen cycle soaking test if the appearance of the test piece is not obviously changed after the test is finished;
the fact that the appearance of the test piece has no obvious change after the test is finished means that after the test is finished, the surface of the test piece is observed by a magnifying lens with the magnification of 10 times, oxidation spots do not appear on the surface, and cracks do not appear on the surface of a coating.
1.2) liquid/gas oxygen flush: flushing is carried out alternately by adopting liquid oxygen and gas oxygen under 0.5MPa, the flushing time is 5-10 min respectively, the appearance of the coating passes through the liquid oxygen/gas oxygen flushing test without obvious change after the test is finished, and the coating passes through the liquid oxygen/gas oxygen flushing test if the appearance of the test piece does not change obviously after the test is finished;
1.3) liquid oxygen mechanical impact test: in the liquid oxygen environment, a punch is adopted to impact the test piece with 98J energy, and 20 test pieces have no flash or 60 test pieces have less than 1 flash, which indicates that the liquid oxygen mechanical impact test is passed.
2) And (3) whole bottle test:
2.1) repeated temperature cycle test: repeatedly soaking at low temperature for 12 times and naturally returning to the temperature (the low temperature is soaked in liquid oxygen at 80K-100K, and the natural temperature is returned to above 293K), and evaluating that the plating passes a repeated temperature cycle test if the plating does not crack or fall off;
2.2) repeated inflation test: and (4) repeatedly inflating and deflating for 12 times, judging that the coating passes a repeated inflation test if the coating does not crack or fall off, and determining the inflation pressure in the repeated inflation test according to the use working condition.
The test piece test and the whole bottle test result meet the requirements, and the coating can meet the reliable application in the liquid oxygen environment.
In the embodiment, the prepared coating test piece test and the whole bottle test result for reducing the impact sensitivity of the titanium alloy gas bottle in the liquid oxygen environment meet the requirements, and the reliable application in the liquid oxygen environment can be met; and the titanium alloy test piece without the coating is adopted to carry out the 98J energy impact test piece, the number of the flash pieces/the number of the test pieces are 3/20 and 5/60 respectively, the titanium alloy test piece with a single copper-plated layer is subjected to 5 times of temperature cycle, the surface of the titanium alloy test piece is subjected to microcrack, the number of the flash pieces/the number of the test pieces are 1/20 and 2/60 respectively, and the reliable application in a liquid oxygen environment cannot be met.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate 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, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (10)
1. A plating layer for reducing the impact sensitivity of a titanium alloy gas cylinder is characterized by comprising a pre-plated nickel layer, a pre-plated copper layer and a copper acid layer which are sequentially plated on the outer surface of the titanium alloy gas cylinder;
the total thickness of the pre-nickel plating layer, the pre-copper plating layer and the acid copper plating layer is recorded as d, the thickness of the pre-nickel plating layer is 60% -75% d, the thickness of the pre-copper plating layer is 15% -25% d, and the thickness of the acid copper plating layer is 5% -20% d.
2. A coating for reducing the impact sensitivity of a titanium alloy gas cylinder according to claim 1, wherein the thickness of the nickel pre-plating layer is 60% d, the thickness of the copper pre-plating layer is 25% d, and the thickness of the copper acid plating layer is 15% d.
3. The method for evaluating the coating is characterized in that when the coating passes a test piece test and a whole bottle test simultaneously, the evaluation of the coating is reliable in a liquid oxygen environment;
the test piece test comprises a liquid oxygen cycle immersion test, a liquid oxygen and gas oxygen scouring test and a liquid oxygen mechanical impact test; the whole bottle test comprises a repeated temperature cycle test and a repeated inflation test;
the specific method of the liquid oxygen cycle immersion test comprises the following steps:
(1.1) soaking the titanium alloy coating test piece in liquid oxygen, taking out and recovering to room temperature;
(1.2) after repeating the step (1.1) for 5-8 times, evaluating that the plating layer passes a liquid oxygen cycle immersion test if the appearance of the test piece has no obvious change;
the specific method of the liquid oxygen and gas oxygen scouring test is as follows: alternately flushing the titanium alloy coating test piece with liquid oxygen and gas oxygen for 5-10 min respectively, and evaluating that the coating passes the liquid oxygen and gas oxygen flushing test if the appearance of the test piece is not obviously changed;
the specific method of 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 through a liquid oxygen mechanical impact test is that no flash exists in more than 20 test pieces or flash is less than 1 in more than 60 test pieces;
the specific method for repeating the 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 step (2.1) is repeated for more than or equal to 2-5 times of the using times of the gas cylinder, evaluating that the plating layer passes a repeated temperature cycle test if the appearance of the plating layer has no obvious change;
the specific method of the repeated inflation test comprises the following steps:
(3.1) inflating the gas cylinder with the titanium alloy coating until the pressure is more than or equal to 1-2 times of the using pressure of the gas cylinder, maintaining the pressure for 1-3 min, and then deflating;
and (3.2) repeating the step (3.1) for more than or equal to 2-5 times of the using times of the gas cylinder, and evaluating that the plating layer passes a repeated inflation test if the appearance of the plating layer does not obviously change.
4. The method according to claim 3, wherein the test piece of the titanium alloy coating layer used in the test piece test is in a disc shape, the diameter of the test piece is 10mm to 15mm, and the thickness of the coating layer of the test piece is calculated according to the following formula:
5. The method for evaluating a plating layer according to claim 3, wherein in the step (1.1) of the liquid oxygen cycle immersion test, the test piece plated with the plating layer is taken out and freely returned to room temperature after being immersed in liquid oxygen for 48 to 72 hours;
the specific method of the liquid oxygen and gas oxygen scouring test is as follows: and (3) alternately flushing the titanium alloy coating test piece with liquid oxygen and gas oxygen at 0.5MPa for 5-10 min respectively, and evaluating that the coating passes the liquid oxygen and gas oxygen flushing test if the appearance of the test piece is not obviously changed.
6. The method 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 scouring tests, the standard of no obvious change of the appearance of the test piece is that the surface of the test piece is observed by a 10-time magnifier, no oxidation spots appear on the surface of the test piece, and no cracks appear on the surface of the coating.
7. The method for evaluating a plating layer according to claim 3, wherein in said repeated thermal cycle test step (2.1), the cylinder is taken out and freely returned to room temperature.
8. The method 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 using the gas cylinder, and the plating is evaluated to pass the temperature cycle test if no obvious change is found in the appearance of the plating;
in the step (3.1) of the repeated inflation test, the gas cylinder plated with the plating layer is inflated until the pressure is equal to 1.5 times of the using pressure of the gas cylinder, and the gas is deflated after the pressure is maintained for 1 min;
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 plating layer is evaluated to pass a repeated inflation test if the appearance of the plating layer is not obviously changed.
9. The method according to claim 3, wherein the criterion of no significant change in appearance of the coating in the repeated thermal cycle test step (2.2) and the repeated inflation test step (3.2) is that no cracks or peeling of the coating surface occurs when the coating surface is observed with a magnifying glass of 10 times.
10. A method of assessing a coating according to any one of claims 3 to 9, wherein the coating is a coating according to claim 1 or 2 for reducing the impact sensitivity of a titanium alloy cylinder.
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