CN110838425B - Three-dimensional carbon array cathode structure modified by metal titanium and preparation method thereof - Google Patents
Three-dimensional carbon array cathode structure modified by metal titanium and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium metal modified three-dimensional carbon array cathode structure and a preparation method thereof, wherein the cathode structure comprises a high-conductivity three-dimensional carbon array, and a titanium metal nano structure is deposited on the surface of the three-dimensional carbon array to form a titanium/three-dimensional carbon array with a core-shell structure; the preparation method of the cathode structure comprises the following steps: 1) preparing a three-dimensional carbon array; 2) ion etching the surface of the three-dimensional carbon array; 3) depositing a metallic titanium layer on the three-dimensional carbon array; 4) and (3) carrying out vacuum annealing on the metallic titanium/three-dimensional carbon array. The cathode structure and the preparation method thereof are not only beneficial to improving the electron emission stability and the emission current density, but also simple in preparation process and low in cost.
Description
Technical Field
The invention relates to the field of vacuum electron field emission, in particular to a three-dimensional carbon array cathode structure modified by metal titanium and a preparation method thereof.
Background
Vacuum electron emission is the process by which electrons are injected into a vacuum from a solid surface. Unlike thermionic emission, cold cathode electron emission requires no heating, and relies only on the action of an electric field to lower the surface barrier height and narrow the width, so that when the barrier width is narrow enough to be comparable to the electron wavelength, electrons tunnel through or over the surface barrier and enter the vacuum. Cold cathodes are widely used in X-ray tubes, microwave devices and optoelectronic devices.
In the aspect of cold cathode materials, Carbon Nanotubes (CNTS), graphene (graphene), and the like have an intrinsically large aspect ratio or width-to-thickness ratio and exhibit a fringe electric field enhancement effect, which can effectively reduce the turn-on and threshold electric fields, thereby improving the field emission performance thereof. However, from the practical application point of view, CNTS and graphene have obstacles to be overcome, such as: (1) the controllable growth of the low-cost large area of the vertical standing substrate; (2) emission point uniformity and stability; (3) the current density needs to be improved.
Disclosure of Invention
The invention aims to provide a titanium metal modified three-dimensional carbon array cathode structure and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a three-dimensional carbon array cathode structure modified by metal titanium comprises a high-conductivity three-dimensional carbon array, wherein a metal titanium nano structure is deposited on the surface of the three-dimensional carbon array to form a titanium/three-dimensional carbon array with a core-shell structure.
The invention also provides a preparation method of the titanium metal modified three-dimensional carbon array cathode structure, which comprises the following steps:
1) preparing a three-dimensional carbon array: processing the cleaned cork into a cuboid, drying, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a tubular furnace with controllable vacuum degree; vacuumizing a tube furnace, introducing high-purity Ar gas into the tube furnace, starting a heating power supply, heating to a set temperature, keeping the temperature for a certain time, and cooling cork to room temperature along with the tube furnace under the protection of the Ar gas to obtain a regularly-arranged three-dimensional carbon array;
2) ion etching of the surface of the three-dimensional carbon array: fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, vacuumizing the coating chamber, then opening a heating system, heating to 150-350 ℃, starting the carrier to rotate, introducing Ar gas into the coating chamber, adjusting the pressure in the coating chamber to be 2.6-3.3 Pa, and applying 400-700V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching;
3) depositing a metallic titanium layer on the three-dimensional carbon array: keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure intensity in the coating chamber to be 0.3-1 Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting a titanium target, and depositing a metal titanium layer on the three-dimensional carbon array;
4) vacuum annealing of the metallic titanium/three-dimensional carbon array: and (3) reducing the vacuum degree in the coating chamber to a set value, heating the temperature in the coating chamber to 500-700 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array to obtain the metal titanium modified three-dimensional carbon array cathode structure.
Further, in the step 1), the cleaned cork is processed into a cuboid with a size of 20mm x 20mm x 5 mm.
Further, in the step 1), drying the cuboid cork wood at 60-90 ℃ for 4-6 hours, then placing the dried cork wood into a ceramic boat, and then placing the ceramic boat containing the cork wood into a tubular furnace with controllable vacuum degree; vacuumizing a tube furnace to be less than 0.1pa, introducing high-purity Ar gas with the flow rate of 200-350 mL/min into the tube furnace, then starting a heating power supply, controlling the heating rate to be less than 1 ℃/min, heating to 900-1100 ℃, preserving heat for 2 hours, and then cooling cork wood to room temperature along with the furnace under the protection of the Ar gas to obtain the regularly arranged three-dimensional carbon array.
Further, in the step 2), after the three-dimensional carbon array is fixed on a carrier of the magnetron sputtering coating chamber, a mechanical pump and a molecular pump are started to vacuumize the coating chamber to be lower than 10 DEG-4And Pa, starting a heating system, heating to 150-350 ℃, starting the carrier to rotate at the rotating speed of 2-8 r/min, introducing 35-50 SCCM of Ar gas into the coating chamber, adjusting the pressure intensity in the coating chamber to be 2.6-3.3 Pa, and applying 400-700V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching for 2-15 min.
Further, in the step 3), the titanium target is started, the target power is 40-100W, a metal titanium layer is deposited on the three-dimensional carbon array for 0.5-10 min to form a metal titanium layer with the thickness of 3-60 nm, and then the titanium target and the Ar air valve are closed.
Further, in the step 3), the vacuum degree in the coating chamber is reduced to be lower than 10-3And Pa, raising the temperature in the coating chamber to 500-700 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array for 30-90 min to obtain the metal titanium modified three-dimensional carbon array cathode structure.
Compared with the prior art, the invention has the following beneficial effects:
1. the environment-friendly cork bark is used as a raw material, the cork bark raw material is directly decomposed to form a three-dimensional orthogonal standing carbon array through a simple pyrolysis process, carbon sheets which are perpendicular to each other in the structure can be used as excellent electron emission units to emit electrons, and the formed hole geometric structure with regular arrangement can effectively reduce the shielding effect of an electric field in vacuum electron field emission;
2. performing Ar ion etching on the three-dimensional carbon skeleton array obtained by high-temperature pyrolysis in a PVD (physical vapor deposition) deposition chamber, so that defects are formed on the surface of the carbon array, electron emission points are increased, and the bonding strength of the deposited titanium/carbon surface is effectively improved;
3. the interface of the carbon and titanium layers forms a titanium carbide structure by adopting a high-temperature vacuum annealing process, and the structure not only improves the bonding strength of the carbon and titanium layers, but also enhances the transport property of electrons at the interface of the carbon and titanium;
4. according to the invention, the three-dimensional carbon array with excellent conductivity is used as a conductive framework, and the metal titanium layer with controllable thickness, excellent conductivity and low work function is deposited and modified on the surface of the three-dimensional carbon array, so that the starting electric field and the threshold electric field of the core-shell cathode array are effectively reduced, and the emission current density and the electron emission stability of the cathode are greatly improved.
Drawings
FIG. 1 is a flow chart of a method of making an embodiment of the present invention.
Fig. 2 is an XRD pattern of the titanium metal/three-dimensional carbon array structure in the example of the present invention.
FIG. 3 is a SEM image of a titanium metal/three-dimensional carbon array structure in an embodiment of the present invention.
Fig. 4 is an EDS spectrum of a titanium metal/three-dimensional carbon array structure in an example of the invention.
FIG. 5 is a diagram of the distribution of carbon and titanium elements in a titanium metal/three-dimensional carbon array structure according to an embodiment of the present invention.
FIG. 6 is a graph of the emission characteristics of the cathode electron field of a three-dimensional carbon array modified by titanium metal with different layer thicknesses in an embodiment of the invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
The invention provides a titanium metal modified three-dimensional carbon array cathode structure which comprises a high-conductivity three-dimensional carbon array, wherein a titanium metal nano structure is deposited on the surface of the three-dimensional carbon array to form a titanium/three-dimensional carbon array with a core-shell structure.
The invention also provides a preparation method of the titanium metal modified three-dimensional carbon array cathode structure, as shown in figure 1, comprising the following steps: 1) preparing a three-dimensional carbon array: processing the cleaned cork into a cuboid, drying, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a tubular furnace with controllable vacuum degree; vacuumizing a tube furnace, introducing high-purity Ar gas into the tube furnace, starting a heating power supply, heating to a set temperature, keeping the temperature for a certain time, and cooling cork to room temperature along with the tube furnace under the protection of the Ar gas to obtain a regularly-arranged three-dimensional carbon array; 2) ion etching of the surface of the three-dimensional carbon array: fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, vacuumizing the coating chamber, then opening a heating system, heating to 150-350 ℃, starting the carrier to rotate, introducing Ar gas into the coating chamber, adjusting the pressure in the coating chamber to be 2.6-3.3 Pa, and applying 400-700V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching; 3) depositing a metallic titanium layer on the three-dimensional carbon array: keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure intensity in the coating chamber to be 0.3-1 Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting a titanium target, and depositing a metal titanium layer on the three-dimensional carbon array; 4) vacuum annealing of the metallic titanium/three-dimensional carbon array: and (3) reducing the vacuum degree in the coating chamber to a set value, heating the temperature in the coating chamber to 500-700 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array to obtain the metal titanium modified three-dimensional carbon array cathode structure.
The invention is further illustrated by the following three specific examples. In the present example, all samples were tested for field emission at a vacuum of 10 degrees-5Pa, the distance between the anode and the cathode is 500um at room temperature. The turn-on voltage is defined as the current density reaching 10 uA/cm2The required voltage value; the threshold voltage is defined as the current density reaching 1mA/cm2The required voltage value.
Example 1
1) Three-dimensional carbon array preparation
Processing cleaned cork into a cuboid with the size of 20mm x 20mm x 5mm, drying at 70 ℃ for 6 hours, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a high-temperature horizontal tube furnace with controllable vacuum degree; vacuumizing the tube furnace to 0.1pa, introducing high-purity Ar gas (99.999) with the flow rate of 300 mL/min into the tube furnace, then starting a heating power supply, controlling the heating rate at 1 ℃/min, heating to 1100 ℃, then preserving heat for 1.5 hours, and then cooling cork wood to room temperature along with the furnace under the protection of the Ar gas to obtain the regularly arranged three-dimensional carbon array.
2) Three-dimensional carbon array surface ion etching
Fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, starting a mechanical pump and a molecular pump to vacuumize the coating chamber to be lower than 10 DEG-4And Pa, then opening a heating system, heating to 200 ℃, starting the carrier to rotate at the rotating speed of 5 r/min, introducing Ar gas 40 SCCM into the coating chamber, adjusting the pressure in the coating chamber to be 2.8 Pa, and applying 600V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching for 5 min.
3) Depositing a metallic titanium layer on a three-dimensional carbon array
Keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure in the coating chamber to be 0.53Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting the titanium target, setting the target power to be 90W, depositing a metal titanium layer on the three-dimensional carbon array for 50 s (seconds) to form a metal titanium layer with the thickness of 5 nm, and then closing the titanium target and the Ar air valve.
4) Vacuum annealing of titanium metal/three-dimensional carbon arrays
The vacuum degree in the film coating chamber is reduced to be less than 10-3Pa, raising the temperature in the coating chamber to 600 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array for 60 min to obtain the metal titanium modificationThe three-dimensional carbon array cathode structure of (1).
The starting voltage of the obtained titanium/three-dimensional carbon array cathode structure is 698V, the threshold voltage is 859V, and the current density reaches 7.34 mA/cm when the voltage is 1097V2。
Example 2
1) Three-dimensional carbon array preparation
Processing cleaned cork into a cuboid with the size of 20mm x 20mm x 5mm, drying at 70 ℃ for 6 hours, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a high-temperature horizontal tube furnace with controllable vacuum degree; vacuumizing the tube furnace to 0.1pa, introducing high-purity Ar gas (99.999) with the flow rate of 300 mL/min into the tube furnace, then starting a heating power supply, controlling the heating rate at 1 ℃/min, heating to 1100 ℃, then preserving heat for 1.5 hours, and then cooling cork wood to room temperature along with the furnace under the protection of the Ar gas to obtain the regularly arranged three-dimensional carbon array.
2) Three-dimensional carbon array surface ion etching
Fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, starting a mechanical pump and a molecular pump to vacuumize the coating chamber to be lower than 10 DEG-4And Pa, then opening a heating system, heating to 200 ℃, starting the carrier to rotate at the rotating speed of 5 r/min, introducing Ar gas 40 SCCM into the coating chamber, adjusting the pressure in the coating chamber to be 2.8 Pa, and applying 600V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching for 5 min.
3) Depositing a metallic titanium layer on a three-dimensional carbon array
Keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure in the coating chamber to be 0.53Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting the titanium target, setting the target power to be 90W, depositing a metal titanium layer on the three-dimensional carbon array for 2.5 min to form a metal titanium layer with the thickness of 15 nm, and then closing the titanium target and the Ar air valve.
4) Vacuum annealing of titanium metal/three-dimensional carbon arrays
The vacuum degree in the film coating chamber is reduced to be less than 10-3Pa, raising the temperature in the coating chamber to 600 ℃ to carry out vacuum annealing on the metallic titanium/three-dimensional carbon arrayAnd (5) obtaining the three-dimensional carbon array cathode structure modified by the metal titanium after 60 min.
The starting voltage of the obtained titanium/three-dimensional carbon array cathode structure is 487V, the threshold voltage is 697V, and the current density reaches 9.76 mA/cm when the voltage is 996V2。
Fig. 2 is an XRD spectrum of the metallic titanium/three-dimensional carbon array structure material synthesized in this example. It can be seen from the figure that 200 corresponds to the metallic titanium peak except the C peak 002, which indicates that the synthesized sample is a titanium/three-dimensional carbon array core-shell nano-structure.
Fig. 3 is an FESEM of the synthesized ti/three-dimensional carbon array structure material of this example. As can be seen, the synthesized titanium/carbon nanostructures are in the form of an array standing orthogonally.
Fig. 4 is an EDS spectrum of the metallic titanium/three-dimensional carbon array structure material synthesized in this example. As can be seen from the figure, the sample elements are mainly composed of C, Ti two elements, indicating that the synthesized sample has high purity.
Fig. 5 is a carbon and titanium distribution diagram of the synthesized titanium/three-dimensional carbon array structure material of this embodiment. From the figure, the metal titanium is uniformly deposited on the surface of the three-dimensional carbon skeleton to form the titanium modified three-dimensional carbon array cathode structure.
Example 3
1) Three-dimensional carbon array preparation
Processing cleaned cork into a cuboid with the size of 20mm x 20mm x 5mm, drying at 70 ℃ for 6 hours, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a high-temperature horizontal tube furnace with controllable vacuum degree; vacuumizing the tube furnace to 0.1pa, introducing high-purity Ar gas (99.999) with the flow rate of 300 mL/min into the tube furnace, then starting a heating power supply, controlling the heating rate at 1 ℃/min, heating to 1100 ℃, then preserving heat for 1.5 hours, and then cooling cork wood to room temperature along with the furnace under the protection of the Ar gas to obtain the regularly arranged three-dimensional carbon array.
2) Three-dimensional carbon array surface ion etching
Fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, and starting a mechanical pump and a molecular pump for counter-platingThe film chamber is vacuumized to be lower than 10 DEG-4And Pa, then opening a heating system, heating to 200 ℃, starting the carrier to rotate at the rotating speed of 5 r/min, introducing Ar gas 40 SCCM into the coating chamber, adjusting the pressure in the coating chamber to be 2.8 Pa, and applying 600V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching for 5 min.
3) Depositing a metallic titanium layer on a three-dimensional carbon array
Keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure in the coating chamber to be 0.53Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting the titanium target, setting the target power to be 90W, depositing a metal titanium layer on the three-dimensional carbon array for 5 min to form a metal titanium layer with the thickness of 30 nm, and then closing the titanium target and the Ar air valve.
4) Vacuum annealing of titanium metal/three-dimensional carbon arrays
The vacuum degree in the film coating chamber is reduced to be less than 10-3And Pa, raising the temperature in the coating chamber to 600 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array for 60 min to obtain the metal titanium modified three-dimensional carbon array cathode structure.
The starting voltage of the obtained titanium/three-dimensional carbon array cathode structure is 1002V, the threshold voltage is 1366V, and the current density reaches 5.82 mA/cm when the voltage is 1785V2。
Fig. 6 is a field electron emission characteristic diagram of the cathode structure material of metallic titanium/three-dimensional carbon array synthesized in example 1, example 2 and example 3. As can be seen, the threshold voltage of the pure three-dimensional carbon array is 1020V, and the current density is 1.8 mA/cm at the maximum when the voltage is 1097V2While the threshold voltages of the materials obtained in example 1, example 2 and example 3 were 859, 697 and 1366V, respectively; the corresponding highest emission current densities reach 7.34, 9.76 and 5.82 mA/cm respectively2。
The above are preferred embodiments of the present invention, and all changes made according to the technical scheme of the present invention that produce functional effects do not exceed the scope of the technical scheme of the present invention belong to the protection scope of the present invention.
Claims (6)
1. A preparation method of a three-dimensional carbon array cathode structure modified by metal titanium is characterized by comprising the following steps:
1) preparing a three-dimensional carbon array: processing the cleaned cork into a cuboid, drying, putting the cork into a ceramic boat, and then putting the ceramic boat containing the cork into a tubular furnace with controllable vacuum degree; vacuumizing a tube furnace, introducing high-purity Ar gas into the tube furnace, starting a heating power supply, heating to a set temperature, keeping the temperature for a certain time, and cooling cork to room temperature along with the tube furnace under the protection of the Ar gas to obtain a regularly-arranged three-dimensional carbon array;
2) ion etching of the surface of the three-dimensional carbon array: fixing the three-dimensional carbon array obtained in the step 1) on a carrier of a magnetron sputtering coating chamber, vacuumizing the coating chamber, then opening a heating system, heating to 150-350 ℃, starting the carrier to rotate, introducing Ar gas into the coating chamber, adjusting the pressure in the coating chamber to be 2.6-3.3 Pa, and applying 400-700V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching;
3) depositing a metallic titanium layer on the three-dimensional carbon array: keeping the working temperature and the rotating speed in the step 2) unchanged, adjusting the pressure intensity in the coating chamber to be 0.3-1 Pa, adjusting the negative bias voltage of the three-dimensional carbon array to be 0V, then starting a titanium target, and depositing a metal titanium layer on the three-dimensional carbon array;
4) vacuum annealing of the metallic titanium/three-dimensional carbon array: and (3) reducing the vacuum degree in the coating chamber to a set value, heating the temperature in the coating chamber to 500-700 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array to obtain the metal titanium modified three-dimensional carbon array cathode structure.
2. The method for preparing a titanium metal modified three-dimensional carbon array cathode structure as claimed in claim 1, wherein in the step 1), the cleaned cork is processed into a cuboid with a size of 20mm x 20mm x 5 mm.
3. The method for preparing a titanium metal modified three-dimensional carbon array cathode structure as claimed in claim 1, wherein in the step 1), a rectangular cork is dried at 60-90 ℃ for 4-6 hours, and then is placed in a ceramic boat, and then the ceramic boat containing the cork is placed in a tube furnace with controllable vacuum degree; vacuumizing a tube furnace to be less than 0.1pa, introducing high-purity Ar gas with the flow rate of 200-350 mL/min into the tube furnace, then starting a heating power supply, controlling the heating rate to be less than 1 ℃/min, heating to 900-1100 ℃, preserving heat for 2 hours, and then cooling cork wood to room temperature along with the furnace under the protection of the Ar gas to obtain the regularly arranged three-dimensional carbon array.
4. The method of claim 1, wherein in step 2), after the three-dimensional carbon array is fixed on a carrier of a magnetron sputtering coating chamber, a mechanical pump and a molecular pump are started to vacuumize the coating chamber to less than 10 degrees centigrade-4And Pa, starting a heating system, heating to 150-350 ℃, starting the carrier to rotate at the rotating speed of 2-8 r/min, introducing 35-50 SCCM of Ar gas into the coating chamber, adjusting the pressure intensity in the coating chamber to be 2.6-3.3 Pa, and applying 400-700V negative bias to the three-dimensional carbon array to enable the surface of the three-dimensional carbon array to be subjected to Ar ion etching for 2-15 min.
5. The method for preparing a titanium-modified three-dimensional carbon array cathode structure as claimed in claim 1, wherein in the step 3), the titanium target is turned on, the target power is 40-100W, the titanium layer is deposited on the three-dimensional carbon array for 0.5-10 min to form a titanium layer with a thickness of 3-60 nm, and then the titanium target and the Ar gas valve are turned off.
6. The method for preparing a titanium metal-modified three-dimensional carbon array cathode structure as claimed in claim 1, wherein in the step 4), the vacuum degree in the coating chamber is reduced to less than 10-3And Pa, raising the temperature in the coating chamber to 500-700 ℃, and carrying out vacuum annealing on the metal titanium/three-dimensional carbon array for 30-90 min to obtain the metal titanium modified three-dimensional carbon array cathode structure.
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