CN103234841B - A kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance - Google Patents
A kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance Download PDFInfo
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Abstract
The present invention relates to a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance, cupping machine is adopted to carry out the test of fibres show creep elongation rate at normal temperatures, invent the feature for superhigh molecular weight polyethylene fibers, by multiple research method, determine the span of creep loading, draw speed, creep time, fiber testing length four test parameters, the creep elongation of test comprises pre-stretched rate and determines load-elongation rate two parts.Compared with prior art, the present invention can characterize preferably to the croop property of different dawn number superhigh molecular weight polyethylene fibers, records creep elongation numerical values recited and is suitable for and good stability.
Description
Technical field
The invention belongs to macromolecular material checking and appraising field, be specifically related to a kind of method of testing superhigh molecular weight polyethylene fibers croop property.
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) fiber is the third generation high-performance fiber occurred after carbon fiber and aramid fiber, and it is with the tygon of relative molecular weight more than 1,000,000 for raw material, and the method through gel spinning-ultra-drawing is prepared from.Be at present specific strength and the highest fiber of ballistic performance in industrialization fibrous material, when equivalent weight, its intensity is equivalent to 15 times of high-quality steel wire.UHMWPE fiber also has excellent chemical resistance and weather resisteant, high-energy absorption, low electric conductivity, can pass through the characteristic such as x-ray and certain water proofing property.Outstanding performance, makes it have broad application prospects in fields such as military affairs, space flight navigation engineering and high-performance, light composite material and sports apparatus.As being used as the flak jackets of protective materials, bulletproof halmet, radar protection cover, guided missile cover, bulletproof armour, stab-resistance body armor and anti-cutting gloves etc.; As the large ship hawser, parachute rope, mine-laying rope, climbing rope etc. of high-strength rope; Make compound substance and be applied to the included wall padded coaming of tank, radome, large-scale storage tank etc.; As the bowstring, canvas, sled etc. of sports apparatus, as optical cable supporting material, setline and fishing net etc.
But, UHMWPE fiber is due to molecular chain length, intermolecular force is little, easily intermolecular slippage is produced under effect of stress, creep is given prominence to, in application process, easily cause the instability of size, form, greatly constrain the application and development of fiber, understand and grasp UHMWPE croop property and be very important.At present, the performance test of UHMWPE fibres show creep only has GB/T19975-2005 " high-strength chemical-fibre filament draw method for testing performance " to do rough introduction.Effective clamping length of this standard regulation test is at least 200mm, apply load and comprise initial load and heavy load, initial load is 0.05cN/dex ± 0.01cN/dex, heavy load is defined as 5%, 10%, 20% of fracture load etc., and load time and heavy load termination time are 1min, 5min, 30min, 1h, 4h, 8h, 24h or extremely rupture.These regulations do not have the scope of exact p-value parameter, particularly do not mention and be loaded into by initial load the sample size change etc. that draw speed in heavy load process and this process occur, its method introduced cannot be adopted to carry out the test of fibres show creep performance.The tensile creep length growth rate mentioned in GB/T19975-2005 standard can not comprise the whole creeps change of fiber in test process, and the numerical values recited of tensile creep length growth rate is not also described, cannot the croop property of the different fiber of Correct.So, the present invention is by various experimental study, determine the numerical value of each parameter in the definition of creep elongation and croop property test process, the creep elongation method of testing formed has test basis, gained creep elongation numerical values recited is suitable, can distinguish the croop property of different model UHMWPE fiber, be conducive to the croop property analyzing the high-intensity fibers such as UHMWPE, to instruct fiber in the application of different occasion.
Summary of the invention
Object of the present invention is exactly that a kind of creep elongation numerical values recited that records in order to overcome that defect that prior art exists provides is suitable for and the method for test superhigh molecular weight polyethylene fibers tensile creep performance of good stability.
Object of the present invention can be achieved through the following technical solutions:
Test a method for superhigh molecular weight polyethylene fibers tensile creep performance, adopt cupping machine to carry out the test of fibres show creep elongation rate at normal temperatures.
Superhigh molecular weight polyethylene fibers can be different manufacturers, model, the superhigh molecular weight polyethylene fibers of dawn number and compound substance thereof.Cupping machine can be any to the stressed stretcher measured with deformation of fiber.
Described creep elongation comprises pre-stretched rate and determines load-elongation rate,
Pre-stretched rate is the length growth rate that superhigh molecular weight polyethylene fibers to be tested produces when initial load arrives creep loading;
Determining load-elongation rate is arrive the length growth rate after creep lotus in creep time.
The detection of described creep elongation comprises the following steps:
(1) by superhigh molecular weight polyethylene fibers to be measured 18 ~ 22 DEG C, humidity at least balances 48h under being the standard atmosphere condition of 62 ~ 68%;
(2) by superhigh molecular weight polyethylene fibers twisting or do not twist process, the fiber of clip testing length, after one end of sample is sandwiched clamper, the other end does not sandwich in another clamper backtwisting;
(3) applying initial load is 0.04 ~ 0.06cN/dex, creep loading is applied gradually under certain draw speed, when arriving creep loading, observe and record the pre-stretched rate of sample, after arriving creep loading, maintain certain creep time, observe and record sample determine load-elongation rate, creep elongation is pre-stretched rate and determine load-elongation rate two sums.
Creep elongation data demand is tested more than 5 times (containing) and is averaged, and the numerical value of mean value is generally greater than 1.0%, CV value and is less than 10%.
Described creep loading is applied to the load on superhigh molecular weight polyethylene fibers when being creep test, the load applied is 10% ~ 60% of fibre breakage load, preferable range is 45 ~ 55% of fibre breakage load, is more preferably 45 ~ 50% of fibre breakage load.
Described draw speed is that fiber is fixed on cupping machine and is loaded into the draw speed in creep loading process by initial load, and the draw speed of employing is 30 ~ 300mm/min, is preferably 100 ~ 200mm/min, is more preferably 120 ~ 150mm/min.
Described creep time is for pointing to the time reached after creep loading set by fiber generation creep elongation, and the creep time of employing is 10 ~ 100min, is preferably 30 ~ 90min, is more preferably 40 ~ 60min.
When described fiber testing length is test, the length of superhigh molecular weight polyethylene fibers is 100 ~ 500mm, is preferably 150 ~ 250mm, is more preferably 200 ~ 250mm.
1), pre-stretched rate, i.e. the sample length growth rate in creep loading this interval from initial load to creep loading creep elongation is divided into two parts by the present invention:; 2), load-elongation rate is determined, the sample length growth rate namely after arrival creep loading in creep time.Wherein, the numerical values recited of size to creep elongation of the during this period of time interior draw speed of creep loading from initial load to creep loading has material impact.
Test method of the present invention is that the UHMWPE fiber sample of test is at least balanced 48h under the standard atmosphere condition of temperature (20 ± 2) DEG C, humidity (65 ± 3) %; According to standard regulation, make under this environmental baseline fiber sample twist (according to test need twisting or do not twist), the testing length of clip fiber, after one end of sample is sandwiched clamper, the other end does not sandwich in another clamper backtwisting.Apply pretension (initial load) 0.05cN/dex ± 0.01cN/dex, after under certain draw speed, apply creep load gradually, creep loading numerical value is 10% of fibre breakage load, 20%, 30%, 40% etc.Arrive before creep loading, observe and record the pre-stretched rate G of sample
0, arrive after creep loading, maintain certain creep time, observe and record sample determine load-elongation rate G
1.The computing formula of creep elongation G is as follows:
G＝G
0+G
1
G
0＝[(l
1-l
0)/l
0]×100％
G
1＝[(l-l
1)/l
1]×100％
In formula:
G-creep elongation, %;
G
0-pre-stretched rate, %;
G
1-Ding load-elongation rate, %;
L
0the initial length of-sample, unit is mm;
L
1-the length of sample when reaching heavy load, unit is mm;
The length of sample after certain creep time after l-heavy load, unit is mm.
According to this method of testing, the inventive method is exceeded molecular weight polyethylene fiber sample to different model and to be tested by single factor and orthogonal test etc., investigate and find creep loading in test process, draw speed, creep time, fiber testing length is the principal element affecting test result, after with creep loading, draw speed, creep time, fiber testing length is independent variable, creep elongation is that dependent variable is chosen representational sample in different model superhigh molecular weight polyethylene fibers and adopted the method for uniform Design to test, the method of linear regression is adopted to process to test result, finally draw the Reasonable Parameters that superhigh molecular weight polyethylene fibers tensile creep rate is tested.By the croop property test parameter chosen, record creep elongation numerical values recited suitable (General Requirements > 1.0%), and stable (General Requirements CV < 10%), show that test result can carry out good comparative analysis to the croop property of different superhigh molecular weight polyethylene fibers.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1-10
Test sample: fiber number is the UHMWPE fiber of 1400D, and fracture strength 27cN/dtex is commercially available.Testing apparatus: DLL-5000 type electronic type puller system, Shanghai De Jie instrument and equipment company limited; Y331A-II type yarn twist meter, Nantong Hongda Experiment Instruments Co., Ltd..Test process: the UHMWPE fiber sample of test is balanced 48h under the standard atmosphere condition of temperature (20 ± 2) DEG C, humidity (65 ± 3) %; The testing length of clip fiber, after one end of sample is sandwiched puller system clamper, the other end also sandwiches in another clamper.Apply pretension (initial load) 0.05cN/dex, after under certain draw speed, apply creep loading gradually, numerical value is respectively 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70% of surveyed fibre breakage load.Arrive before creep loading, observe and record the pre-stretched rate G of sample
0; Arrive after creep loading, maintain certain creep time, observe and record sample determine load-elongation rate.The computing formula of creep elongation G is as follows:
G＝G
0+G
1
G
0＝[(l
1-l
0)/l
0]×100％
G
1＝[(l-l
1)/l
1]×100％
In formula:
G-creep elongation, %;
G
0-pre-stretched rate, %;
G
1-Ding load-elongation rate, %;
L
0the testing length of-sample, unit is mm;
L
1-the length of sample when reaching creep loading, unit is mm;
L-adds the length of sample after certain creep time after creep loading, and unit is mm.
Adopt U
10(10
3× 5) uniform designs table is tested.Table 1 lists uniform designs table and the result thereof of the performance test of UHMWPE fibres show creep.From test result, the creep elongation numerical values recited of fiber is reasonable, the coefficient of variation is generally lower than 10%, but wherein test 7,9,10 when not reaching setting creep time, namely fiber ruptures, not do not complete test according to the experimental factor of design, belong to " catastrophe point ", the result can not tested with other is carried out quadratic polynomial and is returned and process.
The U of table 1UHMWPE fibres show creep performance test
10(10
3× 5) uniform designs table and result thereof
Embodiment 11-16
In Table 1 in test parameter numerical range, select the uniform designs table not making the condition of fibre breakage continue design U6* to test, as shown in table 2, gained test result is reasonable.
The U6* uniform designs table of table 2UHMWPE fibres show creep performance test and result thereof
According to above test figure and test experience, carry out quadratic polynomial successive Regression by effective result of DPS analysis software to twice uniform Design:
Y＝-2.515744413+39.49211852X1*X1+0.000022427802114X4*X4+0.09340136307X1*X3-0.03961365815X1*X4-0.00011008891680X2*X3+0.000031417388347X2*X4
Wherein x1---creep loading, N; X2---draw speed, mm/min; X3---creep time, min; X4---testing length, mm; Y1---creep elongation, %.
Carry out significance test to regression model, as table 3, result shows that regression model can be good at the process of matching croop property test.
The significance test result of table 3 regression model
Draw the croop property test parameter of optimization from regression model, result as table 4,
The combination of each factor of table 4 optimizing index contrasts with test figure
According to the parameter optimized in table 4, for the test of this 1400D superhigh molecular weight polyethylene fibers creep elongation, choose that creep loading is fibre breakage load 50%, draw speed is 200mm/min, creep time is 70min, fiber testing length is 200mm, and gained creep elongation is 7.012%.
Embodiment 17-24
The superhigh molecular weight polyethylene fibers sample choosing different model is tested, as shown in table 5.Testing apparatus: DLL-5000 type electronic type puller system, Shanghai De Jie instrument and equipment company limited; Y331A-II type yarn twist meter, Nantong Hongda Experiment Instruments Co., Ltd..Test process: the UHMWPE fiber sample of test is balanced 48h under the standard atmosphere condition of temperature (20 ± 2) DEG C, humidity (65 ± 3) %; The testing length of clip fiber, after one end of sample is sandwiched puller system clamper, the other end also sandwiches in another clamper.Apply pretension (initial load) 0.05cN/dex, after under certain draw speed, apply creep loading gradually, numerical value is respectively 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50% of fibre breakage load.Arrive before creep loading, observe and record the pre-stretched rate G of sample
0; Arrive after creep loading, maintain certain creep time, observe and record sample determine load-elongation rate G
1.The computing formula of creep elongation G is as follows:
G＝G
0+G
1
G
0＝[(l
1-l
0)/l
0]×100％
G
1＝[(l-l
1)/l
1]×100％
In formula:
G-creep elongation, %;
G
0-pre-stretched rate, %;
G
1-Ding load-elongation rate, %;
L
0the testing length of-sample, unit is mm;
L
1-the length of sample when reaching creep loading, unit is mm;
L-adds the length of sample after certain creep time after creep loading, and unit is mm.
Adopt U
8* uniform designs table is tested, and table 6 lists uniform designs table and test result thereof.
The UHMWPE fiber sample that table 5 is tested
The U of table 6UHMWPE fibres show creep performance test
8* uniform designs table and result thereof
By DPS analysis software, quadratic polynomial successive Regression is carried out to the test findings of uniform Design:
Y＝1.583486928+6.874643127X1+16.833528252X1*X1-0.025360334042X1*X4+0.000017818097413X2*X3+0.0000018190836081X2*X4+0.000013277854719X3*X4
Wherein x1---creep loading, N; X2---draw speed, mm/min; X3---creep time, min; X4---testing length, mm; Y1---creep elongation, %.
Significance test is carried out to regression model, as shown in table 7, show that regression model can be good at the process of matching croop property test.
The significance test result of table 7 regression model
Draw the croop property test parameter of optimization from regression model, result is as shown in table 8.
The croop property test parameter that table 8 is optimized
Embodiment 25-32
According to the croop property test parameter optimized in table 8, in his-and-hers watches 5, the croop property of different dawn number superhigh molecular weight polyethylene fibers sample carries out testing authentication, preferred creep loading is 50% of fibre breakage load, draw speed is 120mm/min, and creep time is 40min, and fiber testing length is 200mm, test result is as shown in table 9, creep elongation size reasonable, CV value < 10%, can the croop property of the sample of evaluation test preferably.
The different dawn number superhigh molecular weight polyethylene fibers croop property of table 9 compares
Embodiment 33
Test sample: add the 1200D superhigh molecular weight polyethylene fibers that 1%wt carbon nano-tube carries out modification, fracture strength 28.3cN/dtex, prepared by laboratory.Testing apparatus: DLL-5000 type electronic type puller system, Shanghai De Jie instrument and equipment company limited; Y331A-II type yarn twist meter, Nantong Hongda Experiment Instruments Co., Ltd..Test process: the UHMWPE fiber sample of test is balanced 48h under the standard atmosphere condition of temperature (20 ± 2) DEG C, humidity (65 ± 3) %; Rear clip fiber test sample 200mm, one end of sample is sandwiched puller system clamper, and the other end also sandwiches in another clamper.Apply pretension (initial load) 0.05cN/dex, after under draw speed 120mm/min, apply creep loading gradually, data by 50% (188.7N) of survey fibre breakage load.Arrive before creep loading, observe and record the pre-stretched rate G of sample
0; Arrive after creep loading and continue 40min, observe and record sample determine load-elongation rate G
1.The computing formula of creep elongation G is as follows:
G＝G
0+G
1
G
0＝[(l
1-l
0)/l
0]×100％
G
1＝[(l-l
1)/l
1]×100％
In formula:
G-creep elongation, %;
G
0-pre-stretched rate, %;
G
1-Ding load-elongation rate, %;
L
0the testing length of-sample, unit is mm;
L
1-the length of sample when reaching creep loading, unit is mm;
L-adds the length of sample after certain creep time after creep loading, and unit is mm.
After tested, the creep elongation calculating this sample is 2.132%.
Claims (14)
1. test the method for superhigh molecular weight polyethylene fibers tensile creep performance for one kind, it is characterized in that, the method adopts cupping machine to carry out the test of fibres show creep elongation rate at normal temperatures, for the feature of superhigh molecular weight polyethylene fibers, by measuring the span of creep loading, draw speed, creep time, fiber testing length four test parameters, the croop property of superhigh molecular weight polyethylene fibers is characterized, detects the numerical value obtaining creep elongation;
Described creep elongation comprises pre-stretched rate and determines load-elongation rate,
Described pre-stretched rate is the length growth rate that superhigh molecular weight polyethylene fibers to be tested produces when initial load arrives creep loading,
Described determines the length growth rate that load-elongation rate is fiber in creep time after arrival creep loading;
The detection of described creep elongation comprises the following steps:
(1) by superhigh molecular weight polyethylene fibers to be measured 18 ~ 22 DEG C, humidity at least balances 48h under being the standard atmosphere condition of 62 ~ 68%;
(2) by superhigh molecular weight polyethylene fibers twisting or do not twist process, the fiber of clip testing length, after one end of sample is sandwiched clamper, the other end does not sandwich in another clamper backtwisting;
(3) applying initial load is 0.04 ~ 0.06cN/dex, creep loading is applied gradually under certain draw speed, when arriving creep loading, observe and record the pre-stretched rate of sample, after arriving creep loading, maintain certain creep time, observe and record sample determine load-elongation rate, creep elongation is pre-stretched rate and determine load-elongation rate two sums.
2. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 1, it is characterized in that, described superhigh molecular weight polyethylene fibers can be different manufacturers, model, the superhigh molecular weight polyethylene fibers of dawn number and compound substance thereof; Cupping machine can be any to the stressed stretcher measured with deformation of fiber.
3. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 1, it is characterized in that, described creep loading is applied to the load on superhigh molecular weight polyethylene fibers when being creep test, the load of applying is 10% ~ 60% of fibre breakage load.
4. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 3, is characterized in that, the load of applying is 45 ~ 55% of fibre breakage load.
5. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 3, is characterized in that, the load of applying is 45 ~ 50% of fibre breakage load.
6. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 1, it is characterized in that, described draw speed is that fiber is fixed on cupping machine and is loaded into the draw speed in creep loading process by initial load, and the draw speed of employing is 30 ~ 300mm/min.
7. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 6, is characterized in that, the draw speed of employing is 100 ~ 200mm/min.
8. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 6, is characterized in that, the draw speed of employing is 100 ~ 120mm/min.
9. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 1, it is characterized in that, described creep time is for pointing to the time reached after creep loading set by fiber generation creep elongation, and the creep time of employing is 10 ~ 100min.
10. a kind of method of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 9, is characterized in that, the creep time of employing is 30 ~ 90min.
11. a kind of methods of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 9, is characterized in that, the creep time of employing is 40 ~ 60min.
12. a kind of methods of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 1, it is characterized in that, during test, the length of superhigh molecular weight polyethylene fibers is 100 ~ 500mm.
13. a kind of methods of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 12, it is characterized in that, during test, the length of superhigh molecular weight polyethylene fibers is 150 ~ 250mm.
14. a kind of methods of testing superhigh molecular weight polyethylene fibers tensile creep performance according to claim 12, it is characterized in that, during test, the length of superhigh molecular weight polyethylene fibers is 200 ~ 250mm.
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| US20180119776A1 (en) * | 2015-05-28 | 2018-05-03 | Dsm Ip Assets B.V. | Polymeric chain link |
| JP6728553B2 (en) * | 2015-05-28 | 2020-07-22 | ディーエスエム アイピー アセッツ ビー．ブイ．Ｄｓｍ Ｉｐ Ａｓｓｅｔｓ Ｂ．Ｖ． | Hybrid chain ring |
| CN104897488A (en) * | 2015-06-05 | 2015-09-09 | 浙江尤夫高新纤维股份有限公司 | Method for testing static creep endurance quality of PET industrial yarns |
| CN104897563A (en) * | 2015-06-18 | 2015-09-09 | 核工业理化工程研究院 | Device and method for measuring creep performance of impregnated fiber yarn |
| CN107255595A (en) * | 2017-06-26 | 2017-10-17 | 安徽长青藤新材料有限公司 | A kind of superhigh molecular weight polyethylene fibers croop property Simplified Test Equipment and method |
| CN109001030B (en) * | 2018-06-28 | 2020-06-26 | 浙江尤夫高新纤维股份有限公司 | Method for testing creep elongation and recovery performance of polyester industrial yarn |
| CN114235555B (en) * | 2021-12-20 | 2024-03-22 | 江苏神韵绳缆有限公司 | Constant load creep testing device for high-modulus polyethylene rope |
| CN114252334A (en) * | 2021-12-20 | 2022-03-29 | 江苏神韵绳缆有限公司 | Method for testing creep performance of high-modulus polyethylene rope |
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| CN101308127A (en) * | 2008-07-08 | 2008-11-19 | 华东理工大学 | Material high-temperature creep life-span accelerated test method |
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