CN110863174A - Titanium-based hydrogen absorption material without activation and preparation method thereof - Google Patents
Titanium-based hydrogen absorption material without activation and preparation method thereof Download PDFInfo
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- CN110863174A CN110863174A CN201911139755.9A CN201911139755A CN110863174A CN 110863174 A CN110863174 A CN 110863174A CN 201911139755 A CN201911139755 A CN 201911139755A CN 110863174 A CN110863174 A CN 110863174A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention belongs to the technical field of getter materials, and relates to a titanium-based hydrogen-absorbing material without activation and a preparation method thereof, wherein the material comprises a gas-absorbing layer, a transition layer and a protective layer, wherein the transition layer and the protective layer are sequentially and symmetrically distributed on two sides of the gas-absorbing layer; the purity of the metal Ti foil in the air suction layer is more than 99.9 percent; the purity of Ti in the transition layer is more than 99.995 percent; the protective layer is any one of Pd, Ni and Pd-Ag alloy, wherein the purity of Pd is more than 99.95%, the purity of Ni is more than 99.995%, and the weight percentage of Ag in the Pd-Ag alloy is 25%. The titanium-based hydrogen absorption material has the characteristics of no need of activation, hydrogen absorption at room temperature, large hydrogen absorption amount, cuttability, adjustable thickness, convenience in use and the like, and can be used for eliminating residual hydrogen of high-vacuum electronic devices and avoiding damage of hydrogen to the devices.
Description
Technical Field
The invention belongs to the technical field of getter materials, and particularly relates to a titanium-based hydrogen absorbing material without activation and a preparation method thereof.
Background
At present, scientific technology and national defense military industry are rapidly developed, and the guarantee of the service life, performance stability and reliability of some key devices becomes a key problem for improving the national defense capability of military in China. Many of the electric vacuum devices currently involved in the vacuum technology field are very sensitive to the internal hydrogen content, for example, gallium arsenide (GaAs) devices in active phased array radar T/R modules, with a small amount of H present inside2Degradation of the sealed device can result; the infrared detector or the solar receiver can be caused by residual H2The presence of (b) results in a severe reduction in its stability and even failure, etc. The hydrogen content inside the device can be effectively controlled by using a material capable of selectively absorbing hydrogen. Thus, has an ideal H2Getter materials with adsorptive properties are considered critical materials in many high vacuum devices. The traditional getter material often has higher surface activity, a layer of passive film is formed on the surface in the process of exposing the atmosphere, and the chemical adsorption and diffusion processes of active gas on the surface of the getter material are blocked, so that the getter material which is not subjected to activation treatment cannot play a gettering role at normal temperature, and the getter material is difficult to be directly applied to a vacuum packaging device with higher requirements on temperature regulation.
Disclosure of Invention
Aiming at the problems, the invention provides a titanium-based hydrogen absorption material without activation and a preparation method thereof, and the specific technical scheme is as follows:
a titanium-based hydrogen absorption material without activation comprises an air absorption layer, a transition layer and a protection layer, wherein the transition layer and the protection layer are sequentially and symmetrically distributed on two sides of the air absorption layer; the purity of the metal Ti foil in the air suction layer is more than 99.9 percent; the purity of Ti in the transition layer is more than 99.995 percent; the protective layer is any one of Pd, Ni and Pd-Ag alloy, wherein the purity of Pd is more than 99.95%, the purity of Ni is more than 99.995%, and the weight percentage of Ag in the Pd-Ag alloy is 25%.
The thickness of the air suction layer is 100-500 mu m; the transition layer is of a compact structure and has the thickness of 100 nm-1 mu m; the protective layer is of a compact structure and has a thickness of 50-500 nm.
A preparation method of a titanium-based hydrogen absorption material without activation comprises the following steps:
1) respectively cleaning the high-purity Ti foil by using acetone, absolute ethyl alcohol and deionized water, and drying by using high-purity argon;
2) removing an oxide layer on the surface of the Ti foil by an ion sputtering method to expose a fresh metal surface of the Ti foil to be used as a getter layer;
3) depositing a Ti film on the getter layer as a transition layer by magnetron sputtering;
4) depositing a Pd film, a Ni film or a Pd-Ag alloy film on the transition layer as a protective layer by magnetron sputtering;
5) turning over the titanium foil, and repeating the steps 2) to 4).
The back bottom of the film coating chamber in the step 2) is vacuumized to 5.0 multiplied by 10-6~5.0×10-4Pa, introducing high-purity argon into the chamber, and bombarding the surface of the Ti foil by ions.
In the step 3), the sputtering pressure is 0.2-1.0 Pa, the sputtering power is 100-300W, the target base distance is 5-8 cm, and the deposition time is 3-30 min.
In the step 4), the sputtering pressure is 0.2-1.0 Pa, the sputtering power is 50-300W, the target base distance is 5-8 cm, and the deposition time is 30-600 s.
The invention has the beneficial effects that:
1. the titanium-based hydrogen absorption material which does not need to be activated has the characteristics of no need of activation, hydrogen absorption at room temperature, large hydrogen absorption amount, cuttability, adjustable thickness, convenience in use and the like, and can be used for eliminating residual hydrogen of high-vacuum electronic devices and avoiding damage of hydrogen to the devices.
Drawings
FIG. 1 is a schematic diagram of the structure of a titanium-based hydrogen absorbing material without activation according to the present invention.
FIG. 2 is a graph showing a static hydrogen absorption performance test of the hydrogen absorption material prepared in examples 1 to 4 at room temperature.
Wherein: 1-a getter layer; 2-a transition layer; 3-protective layer
Detailed Description
A titanium-based hydrogen absorption material without activation is shown in figure 1 and comprises a gas absorption layer 1, a transition layer 2 and a protection layer 3, wherein the transition layer and the protection layer are sequentially and symmetrically distributed on two sides of the gas absorption layer; the two sides of the hydrogen absorbing material are both of a multilayer structure, and the front side and the back side are not distinguished. The purity of the metal Ti foil in the air suction layer is more than 99.9 percent; the purity of Ti in the transition layer is more than 99.995 percent; the protective layer is any one of Pd, Ni and Pd-Ag alloy, wherein the purity of Pd is more than 99.95%, the purity of Ni is more than 99.995%, and the weight percentage of Ag in the Pd-Ag alloy is 25%.
The thickness of the getter layer is 100-500 μm; the transition layer is a compact structure and has the thickness of 100 nm-1 mu m; the protective layer is of a compact structure and has a thickness of 50-500 nm.
A preparation method of a titanium-based hydrogen absorption material without activation comprises the following steps:
1) respectively cleaning the high-purity Ti foil by using acetone, absolute ethyl alcohol and deionized water, and drying by using high-purity argon;
2) removing an oxide layer on the surface of the Ti foil by an ion sputtering method to expose a fresh metal surface of the Ti foil to be used as a getter layer; vacuum pumping the back of the coating chamber to 5.0 × 10-6~5.0×10-4Pa, introducing high-purity argon into the chamber, and bombarding the surface of the Ti foil by ions.
3) Depositing a Ti film on the getter layer as a transition layer by magnetron sputtering; the sputtering pressure is 0.2-1.0 Pa, the sputtering power is 100-300W, the target base distance is 5-8 cm, and the deposition time is 3-30 min.
4) Depositing a Pd film, a Ni film or a Pd-Ag alloy film on the transition layer as a protective layer by magnetron sputtering; the sputtering pressure is 0.2-1.0 Pa, the sputtering power is 50-300W, the target base distance is 5-8 cm, and the deposition time is 30-600 s.
5) Turning over the titanium foil, and repeating the steps 2) to 4).
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
The selective hydrogen absorption material with a double-sided three-layer structure and a Pd membrane as a protective layer is prepared by a magnetron sputtering method by the following steps:
1) sequentially ultrasonically cleaning the Ti foil for 5-15 min by using acetone, absolute ethyl alcohol and high-purity argon, and drying by blowing;
2) removing oxide layer on metal surface by reverse sputtering, putting cleaned Ti foil into coating chamber, starting mechanical pump and molecular pump to vacuumize the back to 5.0 × 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, and adjusting the sputtering pressure to be 0.5Pa for 30 min;
3) preparing a film by adopting a magnetron sputtering method, putting the Ti foil with the oxide layer removed by reverse sputtering into a coating cavity through a sample chamber, and mounting a Ti metal target and a Pd metal target on corresponding target positions; continuing to vacuumize the back to 5.0X 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, adjusting the sputtering pressure to be 3Pa, and pre-sputtering for 15min to ensure that an oxide layer on the surface of the Ti target material is removed; regulating the sputtering pressure to be 0.2Pa, the sputtering power to be 250W, the target base distance to be 7cm and the deposition time to be 20min to form a compact Ti film transition layer;
4) the sputtering pressure is still 0.2Pa, and the Pd target material is pre-sputtered for 2 min; regulating the sputtering power to 150W, the target base distance to 6cm and the deposition time to 150s to form a compact Pd film protective layer;
5) turning over the Ti foil, and repeating the steps 2) to 4).
The thickness of the transition layer of the hydrogen evolution material Ti film prepared in the embodiment 1 is 500nm, and the transition layer is a compact structure; the thickness of the Pd protective layer is 200nm, and the Pd protective layer is of a compact structure. The hydrogen absorption material prepared in example 1 as shown in fig. 2 is a static hydrogen absorption performance test curve under room temperature conditions.
Example 2
Preparing a hydrogen absorption material with a double-layer structure only comprising an air absorption layer and a transition layer by a magnetron sputtering method according to the following steps:
1) sequentially ultrasonically cleaning the Ti foil for 5-15 min by using acetone, absolute ethyl alcohol and high-purity argon, and drying by blowing;
2) by reversingRemoving oxide layer on metal surface by sputtering method, putting cleaned Ti foil into coating chamber, starting mechanical pump and molecular pump to vacuumize back bottom to 5.0 × 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, and adjusting the sputtering pressure to be 0.5Pa for 30 min;
3) preparing a film by adopting a magnetron sputtering method, putting the Ti foil with the oxide layer removed by reverse sputtering into a coating cavity through a sample chamber, and mounting a Ti metal target material on a corresponding target position; continuing to vacuumize the back to 5.0X 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, adjusting the sputtering pressure to be 3Pa, and pre-sputtering for 15min to ensure that an oxide layer on the surface of the Ti target material is removed; regulating the sputtering pressure to be 0.2Pa, the sputtering power to be 250W, the target base distance to be 7cm and the deposition time to be 20min to form a compact Ti film transition layer;
4) turning over the Ti foil, and repeating the steps 2) to 3).
The Ti thin film transition layer prepared in example 2 has a thickness of 500nm and a dense structure. The hydrogen absorption material prepared in example 2 as shown in fig. 2 has a static hydrogen absorption performance test curve under room temperature conditions.
Example 3
The selective hydrogen absorption material with the protective layer being the Pd membrane is prepared by a magnetron sputtering method by adopting the following steps:
1) sequentially ultrasonically cleaning the Ti foil for 5-15 min by using acetone, absolute ethyl alcohol and high-purity argon, and drying by blowing;
2) removing oxide layer on metal surface by reverse sputtering, putting cleaned Ti foil into coating chamber, starting mechanical pump and molecular pump to vacuumize the back to 5.0 × 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, and adjusting the sputtering pressure to be 0.5Pa for 30 min;
3) preparing a film by adopting a magnetron sputtering method, putting the Ti foil with the oxide layer removed by reverse sputtering into a coating cavity through a sample chamber, and mounting a Pd metal target material on a corresponding target position; continuing to vacuumize the back to 5.0X 10-6~5.0×10-4Pa, introducing pure water into the chamberHigh-purity argon with the purity of 99.99999 percent, the sputtering pressure is adjusted to be 0.2Pa, and the Pd target material is pre-sputtered for 2 min; the sputtering pressure is unchanged, the sputtering power is adjusted to be 150W, the target base distance is 6cm, the deposition time is 150s, and a compact Pd thin film protective layer is formed;
4) turning over the Ti foil, and repeating the steps 2) to 3).
The Pd protective layer prepared in example 3 had a thickness of 200nm and was a dense structure. The hydrogen absorption material prepared in example 3 as shown in fig. 2 has a static hydrogen absorption performance test curve under room temperature conditions.
Example 4
The selective hydrogen absorption material with the protective layer of a single-side three-layer structure of the Pd membrane is prepared by a magnetron sputtering method by adopting the following steps:
1) sequentially ultrasonically cleaning the Ti foil for 5-15 min by using acetone, absolute ethyl alcohol and high-purity argon, and drying by blowing;
2) removing oxide layer on metal surface by reverse sputtering, putting cleaned Ti foil into coating chamber, starting mechanical pump and molecular pump to vacuumize the back to 5.0 × 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, and adjusting the sputtering pressure to be 0.5Pa for 30 min;
3) preparing a film by adopting a magnetron sputtering method, putting the Ti foil with the oxide layer removed by reverse sputtering into a coating cavity through a sample chamber, and mounting a Ti metal target and a Pd metal target on corresponding target positions; continuing to vacuumize the back to 5.0X 10-6~5.0×10-4Pa, introducing high-purity argon with the purity of 99.99999 percent into the chamber, adjusting the sputtering pressure to be 3Pa, and pre-sputtering for 15min to ensure that an oxide layer on the surface of the Ti target material is removed; regulating the sputtering pressure to be 0.2Pa, the sputtering power to be 250W, the target base distance to be 7cm and the deposition time to be 20min to form a compact Ti film transition layer;
4) the sputtering pressure is still 0.2Pa, and the Pd target material is pre-sputtered for 2 min; the sputtering power is adjusted to be 150W, the target base distance is 6cm, the deposition time is 150s, and a compact Pd film protective layer is formed.
The thickness of the Ti film transition layer prepared in the embodiment 4 is 500nm, and the Ti film transition layer is of a compact structure; the thickness of the Pd protective layer is 200nm, and the Pd protective layer is of a compact structure. The hydrogen absorption material prepared in example 4 as shown in fig. 2 has a static hydrogen absorption performance test curve under room temperature conditions.
Claims (6)
1. The titanium-based hydrogen absorption material without activation is characterized by comprising a gas absorption layer, a transition layer and a protective layer, wherein the transition layer and the protective layer are sequentially and symmetrically distributed on two sides of the gas absorption layer; the purity of the metal Ti foil in the air suction layer is more than 99.9 percent; the purity of Ti in the transition layer is more than 99.995 percent; the protective layer is any one of Pd, Ni and Pd-Ag alloy, wherein the purity of Pd is more than 99.95%, the purity of Ni is more than 99.995%, and the weight percentage of Ag in the Pd-Ag alloy is 25%.
2. The non-activated titanium-based hydrogen absorbing material as claimed in claim 1, wherein the thickness of the getter layer is 100-500 μm; the transition layer is of a compact structure and has the thickness of 100 nm-1 mu m; the protective layer is of a compact structure and has a thickness of 50-500 nm.
3. A method for preparing a titanium-based hydrogen absorbing material without activation according to claim 1 or 2, comprising the steps of:
1) respectively cleaning the high-purity Ti foil by using acetone, absolute ethyl alcohol and deionized water, and drying by using high-purity argon;
2) removing an oxide layer on the surface of the Ti foil by an ion sputtering method to expose a fresh metal surface of the Ti foil to be used as a getter layer;
3) depositing a Ti film on the getter layer as a transition layer by magnetron sputtering;
4) depositing a Pd film, a Ni film or a Pd-Ag alloy film on the transition layer as a protective layer by magnetron sputtering;
5) turning over the titanium foil, and repeating the steps 2) to 4).
4. The method according to claim 3, wherein the back of the coating chamber in step 2) is vacuumized to 5.0 x 10-6~5.0×10-4Pa, introducing high-purity argon into the chamber, and bombarding the surface of the Ti foil by ions.
5. The method according to claim 3, wherein the sputtering pressure in step 3) is 0.2 to 1.0Pa, the sputtering power is 100 to 300W, the target base distance is 5 to 8cm, and the deposition time is 3 to 30 min.
6. The method according to claim 3, wherein the sputtering pressure in step 4) is 0.2 to 1.0Pa, the sputtering power is 50 to 300W, the target base distance is 5 to 8cm, and the deposition time is 30 to 600 s.
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CN111892014A (en) * | 2020-07-30 | 2020-11-06 | 钢铁研究总院 | Getter film and preparation method thereof |
CN114182205A (en) * | 2021-12-10 | 2022-03-15 | 中国工程物理研究院材料研究所 | Nano multilayer structure metal hydrogen absorption film and preparation method and application thereof |
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