Multilayer titanium film
Technical Field
The utility model belongs to the technical field of novel material, especially, relate to a multilayer titanium membrane.
Background
With the rapid development of composite material technology, novel functional materials and devices are also developed towards miniaturization, integration and compounding, and the research and development of multilayer films are also the key direction of scientific research of novel materials. The multilayer film is a thin film material with alternately changed components or structures, which is formed by alternately depositing different materials. At present, multilayer films with high strength, high toughness, high resistance and high stability are prepared by methods such as ion plating, magnetron sputtering, ion beam assisted deposition, chemical vapor deposition, plasma enhanced chemical vapor deposition, electroplating and the like. The composite film with the multilayer structure shows a series of unique physical, chemical and mechanical properties due to the size, the quality and the particularity of an internal interface, can obviously improve the hardness, the toughness, the wear resistance and the high-temperature oxidation resistance of the surface of a material, effectively reduces the friction and the wear of the surface of the material, and prolongs the service life. Meanwhile, the mutual alternation of the multiple layers of films ensures that the films have a certain hole sealing effect, thereby improving the corrosion resistance of the multiple layers of films. The multi-layer film obviously improves the hardness and toughness of the film, and compared with a single-layer film, the stability and the wear resistance of the multi-layer film are obviously improved.
Titanium is a rare element, has good mechanical properties and strength, is widely applied to the fields of aviation, aerospace, vehicle engineering, biomedical engineering and the like, and a titanium film is mainly applied to the fields of vehicle engineering and biomedicine at present as an ultrathin titanium material. The existing titanium film generally adopts a normal-temperature direct-current magnetron sputtering method to deposit a pure titanium film on the surface of nickel-free stainless steel or other base materials, and a single-layer film is formed at one time; however, in some specific fields, if the thickness of the metallic titanium layer on the surface of the titanium film is in the nanometer level, the surface brittleness of the metallic film layer is increased, and the conductive stability of the metallic film layer is further affected. .
SUMMERY OF THE UTILITY MODEL
One of the purposes of the present invention is to overcome the problems of the prior art by providing a multi-layer titanium film with stronger toughness and more stable surface conductivity.
In order to achieve the above object, the present invention adopts a technical solution including the following aspects.
A multilayer titanium film comprising: the metal layer is attached to the base material, the base material is an insulating plastic film, and the thickness of the base material is 0.5-15 microns; the metal layers comprise a first metal layer, a second metal layer and a third metal layer, and the first metal layer, the second metal layer and the third metal layer are all realized by adopting metal titanium; the thickness of the first metal layer is 30-50 nm, and the first metal layer is attached to the base material insulating plastic film; the thickness of the second metal layer is 70-120 nm, and the second metal layer is attached to the first metal layer; the thickness of the third metal layer is 30-50 nm, and the third metal layer is attached to the second metal layer.
Furthermore, the thickness of the first metal layer is 40nm, the thickness of the second metal layer is 100nm, and the thickness of the third metal layer is 40 nm.
Furthermore, the insulating plastic film comprises a PP polypropylene plastic film, a PET polyterephthalic acid plastic film, a PVC polyvinyl chloride plastic film, a PE polyethylene plastic film, a PU polyurethane plastic film and a TPU thermoplastic polyurethane plastic film.
Furthermore, the insulating plastic layer adopts 1~6 um's PET to make the terephthalic acid plastic film realize, specifically, like 1.5 um's PET film, 4.55 um's PET film.
In conclusion, owing to adopted above-mentioned technical scheme, the utility model discloses following beneficial effect has at least:
the pure titanium multilayer film formed by three times of sputtering has the mechanical properties of high toughness, high tolerance and high stability of the common multilayer film, and the film has stronger toughness compared with a single-layer film with the same thickness through a thin-thick-thin structural form; when the material is applied to the field of biomedicine, the material not only has flexibility and toughness, but also has more stable conductivity.
Drawings
Fig. 1 is a schematic cross-sectional view of a multilayer titanium film according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for preparing a multilayer titanium film according to an embodiment of the present invention.
Fig. 3 is a schematic cross-sectional view of a multilayer titanium film after an annealing process according to an embodiment of the present invention.
Fig. 4 is a schematic drawing of a tensile curve of a multilayer titanium film according to an embodiment of the present invention.
Fig. 5 is a schematic drawing of a tensile curve of a multilayer titanium film according to another embodiment of the present invention.
Fig. 6 is a schematic drawing of a tensile curve of a multilayer titanium film according to another embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and embodiments, so that the objects, technical solutions and advantages of the present invention will be more clearly understood. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
The utility model relates to a multilayer titanium membrane, as shown in figure 1, include: the metal-clad plate comprises a base material 1 and a metal layer attached to the base material 1, wherein the base material is an insulating plastic film, and the thickness of the base material is 0.5-15 microns; the metal layers comprise a first metal layer 21, a second metal layer 22 and a third metal layer 23, and the first metal layer 21, the second metal layer 22 and the third metal layer 23 are all realized by adopting metal titanium; the thickness of the first metal layer 21 is 30-50 nm, and the first metal layer is attached to the base material insulating plastic film 1; the thickness of the second metal layer 22 is 70-120 nm, and the second metal layer 22 is attached to the first metal layer 21; the thickness of the third metal layer 23 is 30-50 nm, and the third metal layer 23 is attached to the second metal layer 22. The utility model discloses form the three-layer metal titanium layer of thin-thick-thin structural style on substrate 1 to form the density for dredging-dense-sparse gradual change formula multilayer film, compare in the same with current substrate, its toughness of the same individual layer titanium membrane of thickness is stronger, stability is higher, can stretch many times and convert into the combination that keeps between the metal titanium layer in the use, guarantee rete surface conductivity.
In the present invention, the thickness of the three metal titanium layers of the multi-layer titanium film is set to be thin-thick-thin, for example, the thickness of the first metal layer is 40nm, the thickness of the second metal layer is 100nm, and the thickness of the third metal layer is 40 nm. Or the thickness of the first metal layer is 30nm, the thickness of the second metal layer is 70nm, and the thickness of the third metal layer is 30 nm. Work as the thickness of first metal level is 40nm, and the thickness of second metal level is 100nm, and the thickness of third metal level is during 40 nm's structural style, and the substrate adopts the PET of 4.55um thickness to make up the terephthalic acid plastic film, and toughness and stability on multilayer titanium membrane surface are optimal, consequently the utility model discloses the preferred thickness that adopts first metal level is 40nm, and the thickness of second metal level is 100nm, and the thickness of third metal level is 40 nm's structural style to and 1~6um PET makes up terephthalic acid plastic film as the substrate.
The insulating plastic film comprises a PP polypropylene plastic film, a PET polyterephthalic acid plastic film, a PVC polyvinyl chloride plastic film, a PE polyethylene plastic film, a PU polyurethane plastic film, a TPU thermoplastic polyurethane plastic film and the like. In order to extensively be applicable to the biomedical field, the utility model discloses in preferably adopt PET to make the base material of PET polyterephthalic acid plastic film as multilayer titanium membrane, thickness is preferably 1~6 um.
Another objective of the present invention is to provide a method for preparing the multilayer titanium film, which combines the simple apparatus diagram shown in fig. 2, and comprises the following steps:
s1, putting the substrate film into the unwinding roller 11 of the winding system, and setting each parameter value of the winding system;
s2, cleaning the substrate film by plasma before the substrate 1 enters the coating functional area, and conveying the substrate film into a coating vacuum chamber after the substrate film is cleaned and attached to the cooling roller 12;
s3, filling argon into the coating vacuum chamber 2, adjusting the vacuum degree, and setting the power of the first magnetron sputtering target 3, the power of the second magnetron sputtering target 4 and the power of the third magnetron sputtering target 5; the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 all adopt titanium with the purity not lower than 99 percent as target sources;
s4, forming metal titanium layers with the thicknesses of 30-50 nm, 70-120 nm and 30-50 nm on the film of the substrate 1 through the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 respectively;
s5, the film after the sputtering of the three metal titanium layers enters an annealing operation area along with the cooling roller 12;
s6, winding the annealed titanium film to a winding roller 13 of a winding system;
and S7, closing the target source, recovering the vacuum chamber 2 to the atmospheric pressure, and taking out the finished multilayer titanium film from the winding system.
The method sets three targets to complete three-layer coating by adopting a winding type coating process, has simple process and can realize large-scale industrial production and application. And forming metal titanium layers with different thicknesses by adjusting the power of each target, thereby completing the multilayer titanium films with different thicknesses. The roll-to-roll process is a well-established process in the prior art, and in the present invention, because the thickness of the substrate is relatively thin, in the embodiment of the present invention, all substrates need to be subjected to a film coating operation before step S1 to ensure that the substrate film is not damaged in the film coating operation.
Magnetron sputtering is a mature coating process, the sputtering rate is improved by applying a magnetic field on the surface of a target to restrict the motion track of charged particles, and the magnetron sputtering method has the advantages of simplicity, high efficiency, high speed, low temperature, low damage and the like. In the utility model, in order to improve the sputtering rate, the first magnetron sputtering target, the second magnetron sputtering target and the third magnetron sputtering target all adopt plane magnetron sputtering targets.
The step S4 can be completed by one of methods of dc magnetron sputtering, intermediate frequency magnetron sputtering, radio frequency magnetron sputtering, and pulse magnetron sputtering.
In order to form a metal titanium layer with a thickness of 30-50 nm, 70-120 nm, 30-50 nm, the power of the first magnetron sputtering target is set to 0.3 kw-0.6 kw, the power of the second magnetron sputtering target is set to 0.8 kw-1.4 kw, and the power of the third magnetron sputtering target is set to 0.3 kw-0.6 kw.
In the steps S5 and S6, the annealing operation is a metal heat treatment process of reheating the cooled film to a predetermined temperature, keeping the temperature for a certain time, and then slowly cooling, which is a common process in the prior art; apply annealing process in the utility model discloses in the preparation method, obvious interface between the three-layer membrane structure can effectively be eliminated to control annealing temperature and time, as shown in fig. 3, improves the contact surface stress between the three-layer metal titanium layer, makes it fuse to overall structure to form the density for sparse-dense-sparse gradual change formula multilayer film, improve the toughness of film and the stability of surface conductivity.
Example 1
S1, adopting a TPU plastic film with the thickness of 12.5um as a base material 1, putting the base material film into an unwinding roller 11 in a winding system, setting various parameter values of the winding system, wherein the transmission speed is set to be 3m/min, and the tension among the unwinding roller 11, a cooling roller 12, a winding roller 13 and a passing roller 14 is controlled to be about 280N;
s2, cleaning the substrate film by plasma before the substrate 1 enters the coating functional area, and conveying the substrate film attached to the cooling roller 12 into the coating vacuum chamber 2 after the substrate film is cleaned;
s3, filling 30sccm argon gas into the film coating vacuum chamber 2, adjusting the vacuum degree to be 0.15Pa, and setting the power of the first magnetron sputtering target 3 to be 0.5kw, the power of the second magnetron sputtering target 4 to be 1kw, and the power of the third magnetron sputtering target 5 to be 0.5 kw; the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 all adopt titanium with the purity not lower than 99 percent as a plane target source;
s4, forming metal titanium layers with the thicknesses of 50nm, 90nm and 50nm on the substrate 1 through the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 respectively;
s5, enabling the film after the three-layer metal titanium sputtering is finished to enter an annealing operation area along with the cooling roller 12, setting the annealing temperature to be 120 ℃ and the annealing time to be 5 h;
s6, winding the annealed titanium film to a winding roller 13 of a winding system;
and S7, closing the target source, recovering the vacuum chamber to the atmospheric pressure, and taking out the finished multilayer titanium film from the winding system.
The total thickness of the multilayer titanium film formed by the method of the embodiment is about 12.7 um; randomly selecting any part of the film, cutting the film into dumbbell-shaped samples, and performing tensile test on the cut samples by adopting a film tensile property test method in the prior art, wherein the test data of one sample is shown in table 1, and a corresponding tensile curve diagram is shown in fig. 4:
watch 1
Tension force
|
Strain of
|
Stress
|
Tension force
|
Strain of
|
Stress
|
(N)
|
(mm)
|
(Mpa)
|
(N)
|
(mm)
|
(Mpa)
|
0.0032
|
0.7924
|
0.1283
|
3.1029
|
4.7329
|
123.6206
|
0.0101
|
0.7948
|
0.4007
|
3.1042
|
4.7346
|
123.6735
|
0.0737
|
1.0788
|
2.9357
|
3.1165
|
4.8148
|
124.1649
|
0.7391
|
1.2499
|
29.4464
|
3.1169
|
4.8193
|
124.1799
|
0.7588
|
1.2528
|
30.2303
|
3.1370
|
4.9393
|
124.9808
|
0.7801
|
1.2548
|
31.0802
|
3.1378
|
4.9425
|
125.0107
|
0.8023
|
1.2595
|
31.9656
|
3.1381
|
4.9444
|
125.0235
|
0.8411
|
1.2644
|
33.5097
|
3.1634
|
5.1044
|
126.0300
|
0.8569
|
1.2690
|
34.1414
|
3.1630
|
5.1089
|
126.0172
|
1.1928
|
1.3328
|
47.5220
|
3.2434
|
5.4223
|
129.2193
|
1.2066
|
1.3348
|
48.0719
|
3.2769
|
5.6100
|
130.5541
|
1.6585
|
1.4290
|
66.0747
|
3.3787
|
6.1089
|
134.6080
|
1.6882
|
1.4346
|
67.2602
|
3.3979
|
6.2146
|
135.3749
|
1.7740
|
1.4690
|
70.6768
|
3.4162
|
6.3249
|
136.1035
|
2.1210
|
1.5651
|
84.5035
|
3.4166
|
6.3298
|
136.1205
|
2.1334
|
1.5700
|
84.9973
|
3.4177
|
6.3330
|
136.1627
|
2.1448
|
1.5726
|
85.4495
|
3.4201
|
6.3393
|
136.2571
|
2.1548
|
1.5746
|
85.8475
|
3.4203
|
6.3548
|
136.2671
|
2.1650
|
1.5794
|
86.2530
|
3.4201
|
6.3588
|
136.2609
|
2.2327
|
1.6126
|
88.9531
|
3.4324
|
6.4450
|
136.7470
|
2.2408
|
1.6146
|
89.2766
|
3.4329
|
6.4499
|
136.7704
|
2.2701
|
1.6244
|
90.4436
|
3.4339
|
6.4530
|
136.8095
|
2.3304
|
1.6690
|
92.8427
|
3.4587
|
6.5793
|
137.7958
|
2.3566
|
1.7091
|
93.8873
|
3.4596
|
6.5844
|
137.8310
|
2.3910
|
1.7250
|
95.2575
|
3.4253
|
6.5924
|
136.4655
|
2.4398
|
1.7698
|
97.2038
|
3.2950
|
6.5949
|
131.2747
|
2.4555
|
1.8223
|
97.8298
|
3.0539
|
6.5988
|
121.6680
|
2.4603
|
1.8243
|
98.0202
|
2.8343
|
6.6030
|
112.9206
|
2.5005
|
1.9548
|
99.6205
|
2.7411
|
6.6050
|
109.2062
|
2.5007
|
1.9890
|
99.6279
|
2.6967
|
6.6098
|
107.4400
|
2.5009
|
2.0223
|
99.6356
|
2.6128
|
6.6130
|
104.0951
|
2.5643
|
2.3124
|
102.1647
|
2.5155
|
6.6146
|
100.2178
|
2.6050
|
2.4348
|
103.7836
|
2.4436
|
6.6193
|
97.3533
|
2.6047
|
2.4388
|
103.7726
|
2.3931
|
6.6225
|
95.3420
|
2.6373
|
2.6788
|
105.0722
|
2.3553
|
6.6244
|
93.8348
|
2.6383
|
2.6830
|
105.1122
|
2.3336
|
6.6286
|
92.9715
|
2.6980
|
2.9588
|
107.4891
|
2.4108
|
6.6430
|
96.0494
|
2.7597
|
3.1628
|
109.9495
|
2.4300
|
6.6449
|
96.8113
|
2.7734
|
3.2223
|
110.4922
|
2.4702
|
6.6548
|
98.4144
|
2.7737
|
3.2243
|
110.5051
|
2.4684
|
6.6896
|
98.3408
|
2.7854
|
3.2850
|
110.9736
|
2.5015
|
6.6948
|
99.6626
|
2.7861
|
3.2898
|
111.0008
|
2.5240
|
6.6993
|
100.5581
|
2.7872
|
3.2928
|
111.0429
|
2.5479
|
6.7026
|
101.5113
|
2.8636
|
3.7650
|
114.0890
|
2.5931
|
6.7089
|
103.3119
|
2.8675
|
3.7699
|
114.2433
|
2.2669
|
6.7630
|
90.3143
|
2.9106
|
3.8450
|
115.9594
|
2.2872
|
6.7649
|
91.1221
|
2.9128
|
3.8499
|
116.0472
|
2.3268
|
6.7730
|
92.7006
|
2.9705
|
4.1748
|
118.3473
|
2.3657
|
6.7793
|
94.2494
|
2.9694
|
4.1793
|
118.3030
|
2.4186
|
6.7889
|
96.3566
|
2.9677
|
4.1824
|
118.2338
|
2.4342
|
6.7925
|
96.9784
|
2.9594
|
4.2348
|
117.9027
|
2.4498
|
6.7949
|
97.6011
|
2.9968
|
4.4098
|
119.3961
|
2.4657
|
6.7989
|
98.2342
|
3.0201
|
4.5188
|
120.3220
|
2.4974
|
6.8050
|
99.4993
|
3.0216
|
4.5230
|
120.3835
|
2.5127
|
6.8098
|
100.1061
|
3.0643
|
4.5844
|
122.0829
|
2.5288
|
6.8130
|
100.7492
|
3.0646
|
4.5889
|
122.0964
|
2.3231
|
6.8786
|
92.5533
|
3.1014
|
4.7296
|
123.5615
|
2.2053
|
6.9086
|
87.8596 |
According to the experimental data, the average elastic modulus E of the sample is 110.4457MPa, the average breaking strength is 138.43MPa, and the average breaking elongation is 3.3059%.
A single-layer titanium film (a TPU plastic film with a base material of 12.5um and a titanium plating film with the specification of about 200 nm) with the same thickness in the prior art is selected to be subjected to a comparative test according to the test method, so that the sample has the average elastic modulus E of 125.1559MPa, the average breaking strength of 115.24MPa and the average breaking elongation of 2.447 percent. According to the above experimental data, the multilayer titanium film prepared by the method of the utility model not only has increased flexibility, but also has improved toughness of the film surface.
In addition, the number of samples with surface fracture of the multilayer titanium film after 20 parts of the multilayer titanium film with the same size of 15cm multiplied by 15cm and 20 parts of single-layer titanium film samples with the same thickness in the prior art are selected and folded at any position of 20 positions is as follows: 2, the number of samples of the single-layer titanium film with surface fracture is as follows: 9; if the fracture can seriously influence its electric conductive property in the metal film if the surperficial metal level appears, because of the utility model discloses the multilayer titanium membrane of method preparation can effectively guarantee the stability of metal film layer surface conductivity ability.
Example 2
S1, adopting a PET plastic film with the thickness of 4.55um as a base material, putting the base material film 1 into an unwinding roller 11 in a winding system, setting various parameter values of the winding system, wherein the transmission speed is set to be 3m/min, and the tension among the unwinding roller 11, a cooling roller 12, a winding roller 13 and a passing roller 14 is controlled to be about 300N;
s2, cleaning the substrate film by plasma before the substrate enters the coating functional area, and conveying the substrate film attached to the cooling roller 12 into the coating vacuum chamber 2 after the substrate film is cleaned;
s3, filling 30sccm argon gas into the film coating vacuum chamber, adjusting the vacuum degree to be 0.15Pa, and setting the power of the first magnetron sputtering target 3 to be 0.5kw, the power of the second magnetron sputtering target 4 to be 1.2kw and the power of the third magnetron sputtering target 5 to be 0.5 kw; the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 all adopt titanium with the purity not lower than 99 percent as a plane target source;
s4, forming metal titanium layers with the thicknesses of 40nm, 100nm and 40nm on the substrate 1 through the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 respectively;
s5, enabling the film after the three-layer metal titanium sputtering is finished to enter an annealing operation area along with the cooling roller 12, setting the annealing temperature to be 115 ℃ and the annealing time to be 5 h;
s6, winding the annealed titanium film to a winding roller 13 of a winding system;
and S7, closing the target source, recovering the vacuum chamber 2 to the atmospheric pressure, and taking out the finished multilayer titanium film from the winding system.
The total thickness of the multilayer titanium film formed by the method of the embodiment is about 4.7 um; randomly selecting any part of the film to be cut into dumbbell-shaped samples, and performing tensile test on the cut samples by adopting a film tensile property test method in the prior art, wherein the test data of one sample is shown in table 2, and a curve H in a graph 5 is a corresponding tensile curve:
watch two
Tension force
|
Strain of
|
Stress
|
Tension force
|
Strain of
|
Stress
|
(N)
|
(mm)
|
(Mpa)
|
(N)
|
(mm)
|
(Mpa)
|
0.0107
|
0.0124
|
1.1305
|
0.9909
|
0.4788
|
104.3010
|
0.0120
|
0.0140
|
1.2682
|
0.9959
|
0.4830
|
104.8311
|
0.0552
|
0.0721
|
5.8069
|
1.0005
|
0.4850
|
105.3198
|
0.0641
|
0.0829
|
6.7447
|
1.0119
|
0.4929
|
106.5205
|
0.0699
|
0.0850
|
7.3565
|
1.0175
|
0.4946
|
107.1015
|
0.0843
|
0.0929
|
8.8708
|
1.0226
|
0.4991
|
107.6424
|
0.0903
|
0.0946
|
9.5050
|
1.0274
|
0.5025
|
108.1511
|
0.0955
|
0.0994
|
10.0487
|
1.0795
|
0.5548
|
113.6343
|
0.1308
|
0.1230
|
13.7654
|
1.0821
|
0.5589
|
113.9100
|
0.1348
|
0.1250
|
14.1887
|
1.0882
|
0.5650
|
114.5448
|
0.1680
|
0.1489
|
17.6890
|
1.0907
|
0.5699
|
114.8115
|
0.1788
|
0.1548
|
18.8244
|
1.0936
|
0.5730
|
115.1191
|
0.1841
|
0.1589
|
19.3782
|
1.1034
|
0.5844
|
116.1463
|
0.1902
|
0.1629
|
20.0248
|
1.1255
|
0.6225
|
118.4707
|
0.2131
|
0.1729
|
22.4321
|
1.1386
|
0.6530
|
119.8478
|
0.2214
|
0.1748
|
23.3036
|
1.1401
|
0.6546
|
120.0100
|
0.2293
|
0.1794
|
24.1358
|
1.1419
|
0.6591
|
120.2041
|
0.2371
|
0.1825
|
24.9533
|
1.1483
|
0.6786
|
120.8757
|
0.2447
|
0.1844
|
25.7539
|
1.1498
|
0.6830
|
121.0337
|
0.2524
|
0.1889
|
26.5640
|
1.1574
|
0.6993
|
121.8319
|
0.2607
|
0.1924
|
27.4447
|
1.1591
|
0.7025
|
122.0077
|
0.2971
|
0.2050
|
31.2777
|
1.1599
|
0.7044
|
122.0944
|
0.3064
|
0.2098
|
32.2494
|
1.1767
|
0.7630
|
123.8588
|
0.3249
|
0.2146
|
34.1998
|
1.1777
|
0.7650
|
123.9703
|
0.3455
|
0.2225
|
36.3663
|
1.1784
|
0.7698
|
124.0458
|
0.3651
|
0.2288
|
38.4331
|
1.1798
|
0.7730
|
124.1892
|
0.3749
|
0.2323
|
39.4595
|
1.1945
|
0.8288
|
125.7329
|
0.3841
|
0.2346
|
40.4281
|
1.1964
|
0.8450
|
125.9411
|
0.4042
|
0.2430
|
42.5494
|
1.1976
|
0.8498
|
126.0623
|
0.4141
|
0.2450
|
43.5903
|
1.2130
|
0.9123
|
127.6878
|
0.4247
|
0.2499
|
44.7017
|
1.2244
|
0.9729
|
128.8887
|
0.4358
|
0.2529
|
45.8766
|
1.2255
|
0.9746
|
129.0023
|
0.4461
|
0.2548
|
46.9623
|
1.2672
|
1.2028
|
133.3899
|
0.4564
|
0.2593
|
48.0424
|
1.2731
|
1.2321
|
134.0154
|
0.4669
|
0.2625
|
49.1520
|
1.2832
|
1.3148
|
135.0784
|
0.4762
|
0.2644
|
50.1278
|
1.2990
|
1.4126
|
136.7320
|
0.4848
|
0.2688
|
51.0343
|
1.2996
|
1.4146
|
136.8038
|
0.4940
|
0.2724
|
51.9970
|
1.3000
|
1.4195
|
136.8444
|
0.5643
|
0.2948
|
59.3983
|
1.3009
|
1.4223
|
136.9324
|
0.5738
|
0.2993
|
60.4025
|
1.3017
|
1.5044
|
137.0202
|
0.5842
|
0.3025
|
61.4986
|
1.3017
|
1.5091
|
137.0249
|
0.5947
|
0.3044
|
62.5992
|
1.3126
|
1.5890
|
138.1728
|
0.6049
|
0.3089
|
63.6782
|
1.3134
|
1.5920
|
138.2548
|
0.6157
|
0.3124
|
64.8059
|
1.3279
|
1.6926
|
139.7784
|
0.6260
|
0.3148
|
65.8942
|
1.3576
|
1.9023
|
142.9021
|
0.6353
|
0.3188
|
66.8757
|
1.3579
|
1.9044
|
142.9417
|
0.6439
|
0.3230
|
67.7788
|
1.3666
|
1.9889
|
143.8546
|
0.6884
|
0.3393
|
72.4587
|
1.3668
|
1.9948
|
143.8745
|
0.6976
|
0.3425
|
73.4317
|
1.3679
|
2.0028
|
143.9849
|
0.7060
|
0.3444
|
74.3106
|
1.3679
|
2.0049
|
143.9932
|
0.7134
|
0.3488
|
75.0990
|
1.3685
|
2.0098
|
144.0518
|
0.7210
|
0.3523
|
75.8929
|
1.3693
|
2.0128
|
144.1412
|
0.7288
|
0.3548
|
76.7129
|
1.3865
|
2.2430
|
145.9472
|
0.7370
|
0.3588
|
77.5752
|
1.3779
|
2.2830
|
145.0463
|
0.7457
|
0.3630
|
78.4958
|
1.3759
|
2.2849
|
144.8342
|
0.7546
|
0.3650
|
79.4265
|
1.3734
|
2.2896
|
144.5686
|
0.7635
|
0.3698
|
80.3648
|
1.3678
|
2.2929
|
143.9751
|
0.8302
|
0.3949
|
87.3917
|
1.3404
|
2.2948
|
141.0906
|
0.8374
|
0.3988
|
88.1478
|
1.2444
|
2.2993
|
130.9883
|
0.8577
|
0.4098
|
90.2802
|
1.0216
|
2.3025
|
107.5377
|
0.8650
|
0.4129
|
91.0520
|
0.6793
|
2.3045
|
71.5001
|
0.8805
|
0.4193
|
92.6792
|
0.3415
|
2.3090
|
35.9447
|
0.8879
|
0.4225
|
93.4629
|
0.1352
|
2.3123
|
14.2265
|
0.8946
|
0.4244
|
94.1712
|
0.0601
|
2.3148
|
6.3294
|
0.9073
|
0.4324
|
95.5063
|
0.0455
|
2.3189
|
4.7866
|
0.9134
|
0.4348
|
96.1479
|
0.0413
|
2.3230
|
4.3447
|
0.9273
|
0.4430
|
97.6156
|
0.0332
|
2.3250
|
3.4915
|
0.9338
|
0.4449
|
98.2925
|
0.0275
|
2.3298
|
2.8910
|
0.9755
|
0.4688
|
102.6821
|
0.0247
|
2.3330
|
2.6002 |
According to the experimental data, the average elastic modulus E of the sample is 88.1925MPa, the average breaking strength is 144.81MPa, and the average breaking elongation is 1.1255%.
A single-layer titanium film (a PET plastic film with a base material of 4.55um serving as a plastic film and titanium plating with the specification of about 200 nm) with the same thickness in the prior art is selected to be subjected to a comparative test according to the test method, and a curve B in a graph in FIG. 5 is a corresponding tensile curve graph to obtain a sample with the average elastic modulus E of 110.6394MPa, the average breaking strength of 115.176MPa and the average breaking elongation of 0.815 percent. According to the above experimental data, the multilayer titanium film prepared by the method of the utility model not only has increased flexibility, but also has improved toughness of the film surface.
In addition, the number of samples with surface fracture of the multilayer titanium film after 20 parts of the multilayer titanium film with the same size of 15cm multiplied by 15cm and 20 parts of single-layer titanium film samples with the same thickness in the prior art are selected and folded at any position of 20 positions is as follows: 1, the number of samples of the single-layer titanium film with surface fracture is as follows: 7; if the fracture can seriously influence its electric conductive property in the metal film if the surperficial metal level appears, because of the utility model discloses the multilayer titanium membrane of method preparation can effectively guarantee the stability of metal film layer surface conductivity ability.
Example 3
S1, adopting a PET plastic film with the thickness of 1.6 um as a substrate 1, putting the substrate film into an unwinding roller 11 in a winding system, setting various parameter values of the winding system, wherein the transmission speed is set to be 3m/min, and the tension among the unwinding roller 11, a cooling roller 12, a winding roller 13 and a passing roller 14 is controlled to be about 300N;
s2, cleaning the substrate film by plasma before the substrate 1 enters the coating functional area, and conveying the substrate film attached to the cooling roller 12 into the coating vacuum chamber 2 after the substrate film is cleaned;
s3, filling 30sccm argon gas into the film coating vacuum chamber 2, adjusting the vacuum degree to be 0.15Pa, and setting the power of the first magnetron sputtering target 3 to be 0.3kw, the power of the second magnetron sputtering target 4 to be 0.9kw, and the power of the third magnetron sputtering target 5 to be 0.3 kw; the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 all adopt titanium with the purity not lower than 99 percent as a plane target source;
s4, forming metal titanium layers with the thicknesses of 30nm, 80nm and 30nm on the base material through the first magnetron sputtering target 3, the second magnetron sputtering target 4 and the third magnetron sputtering target 5 respectively;
s5, enabling the film after the three-layer metal titanium sputtering is finished to enter an annealing operation area along with the cooling roller 12, setting the annealing temperature to be 120 ℃ and the annealing time to be 5 h;
s6, winding the annealed titanium film to a winding roller 13 of a winding system;
and S7, closing the target source, recovering the vacuum chamber 2 to the atmospheric pressure, and taking out the finished multilayer titanium film from the winding system.
The total thickness of the multilayer titanium film formed by the method of the embodiment is about 1.7 um; randomly selecting any part of the film, cutting the film into dumbbell-shaped samples, and performing tensile test on the cut samples by adopting a film tensile property test method in the prior art, wherein FIG. 6 is a corresponding tensile curve chart; according to the experimental data, the average elastic modulus E of the sample is 83.9505MPa, the average breaking strength is 37.7618MPa, and the average breaking elongation is 0.253 percent.
The above description is only for the purpose of illustrating the embodiments of the present invention, and not for the purpose of limiting the same. Various substitutions, modifications and improvements may be made by those skilled in the relevant art without departing from the spirit and scope of the invention.