High strength vacuum deposited nitinol alloy films and method of making same
View Patent ↗A vacuum deposition method for fabricating high-strength nitinol films by sputter depositing nickel and titanium from a heated sputtering target, and controlling the sputter deposition process parameters in order to create high-strength nitinol films that exhibit shape memory and/or superelastic properties without the need for precipitation annealing to attenuate the transition conditions of the deposited material. A vacuum deposited nitinol film having high-strength properties equal to or better than wrought nitinol films and which are characterized by having non-columnar crystal grain structures.
1. A shape memory nickel-titanium film comprising a seamless tubular structure having a substantially non-columnar crystalline micro structure substantially free of precipitates and an ultimate strength greater than about 500 MPa.
2. The shape memory nickel-titanium film according to claim 1 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 6%.
3. The shape memory nickel-titanium film according to claim 2 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 8%.
4. The shape memory nickel-titanium film according to claim 3 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 10%.
5. The shape memory nickel-titanium film according to claim 4 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 12%.
6. A shape memory nickel-titanium film comprising a seamless tubular structure having a substantially non-colunmar crystalline grain morphology substantially free of precipitates and an ultimate strength greater than about 500 MPa.
7. The shape memory nickel-titanium film according to claim 6 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 6%.
8. The shape memory nickel-titanium film according to claim 7 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 8%.
9. The shape memory nickel-titanium film according to claim 8 , wherein the seamless tubular micro structure exhibits a maximum strain greater than about 10%.
10. The shape memory nickel-titanium film according to claim 9 , wherein the seamless tubular microstructure exhibits a maximum strain greater than about 12%.
11. A nitinol film, comprising a seamless tubular structure having a substantially non-columnar crystalline microstructure substantially free of precipitates, made by sputter depositing nickel-titanium in a vacuum system having a magnetron, a target, a substrate, a cooling device thermally coupled to the cathode and a deposition chamber capable of being selectively isolated from the atmosphere, the improvement comprising: controlling the energy of particles emitted from the target such tat the mean free path of the emitted particles is greater than about one-half of the throw distance between the target and the substrate.
12. The nitinol film according to claim 11 , characterized by having substantially non-columnar crystal grain structures.
13. The nitinol film according to claim 11 , characterized by having an ultimate strength greater than 500 MPa.
14. The nitinol film according to claim 11 , consisting essentially of nickel and titanium.
15. The nitinol film according to claim 11 , characterized by having substantially no precipitates within the nitinol film.
16. A shape memory film, comprising a seamless tubular structure having a substantially non-columnar crystalline microstructure substantially free of precipitates, made by a method comprising the steps of:
a. providing a vacuum deposition apparatus;
b. providing at least one target selected from the group consisting of nickel, titanium, nickel-titanium alloy, nickel-titanium-X alloy wherein X is selected from the group of copper, chromium, tantalum and zirconium;
c. providing and heating a substrate before and during a deposition run;
d. vacuum depositing metal from the at least one target onto the deposition substrate;
e. controlling at least one vacuum deposition processing parameter selected from the group of isothermally heating the deposition target, controlling the base vacuum pressure, deoxygenating the working gas, controlling the deposition pressure, controlling surface roughness of the substrate, controlling the composition of the substrate, applying a negative bias voltage to the substrate and controlling the throw distance between the deposition substrate and the deposition target thereby forming the micro structure substantially free of precipitates; and f. removing the deposited metal from the deposition substrate.
17. The shape memory film of claim 16 , having substantially non-columnar crystal grain morphology and an ultimate strength greater than about 500 MPa.
18. The shape memory film of claim 17 , further comprising a maximum strain greater than about 6%.
19. The shape memory film of claim 16 , consisting essentially of nickel and titanium and without substantial presence of precipitates.