CN114540754A - Cu/Ti-W/ceramic composite material and preparation method thereof - Google Patents
Cu/Ti-W/ceramic composite material and preparation method thereof Download PDFInfo
- Publication number
- CN114540754A CN114540754A CN202210349511.9A CN202210349511A CN114540754A CN 114540754 A CN114540754 A CN 114540754A CN 202210349511 A CN202210349511 A CN 202210349511A CN 114540754 A CN114540754 A CN 114540754A
- Authority
- CN
- China
- Prior art keywords
- composite material
- ceramic composite
- ceramic substrate
- sputtering
- ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 171
- 239000002131 composite material Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000010949 copper Substances 0.000 claims abstract description 99
- 239000000758 substrate Substances 0.000 claims abstract description 84
- 230000007704 transition Effects 0.000 claims abstract description 36
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 30
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010849 ion bombardment Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 116
- 229910052786 argon Inorganic materials 0.000 claims description 58
- 239000013077 target material Substances 0.000 claims description 34
- 229910001080 W alloy Inorganic materials 0.000 claims description 23
- 239000012298 atmosphere Substances 0.000 claims description 19
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 5
- 239000011888 foil Substances 0.000 abstract description 40
- 239000002360 explosive Substances 0.000 abstract description 22
- 239000002184 metal Substances 0.000 abstract description 22
- 229910052751 metal Inorganic materials 0.000 abstract description 22
- 230000008569 process Effects 0.000 abstract description 11
- 239000010409 thin film Substances 0.000 abstract description 10
- 238000001259 photo etching Methods 0.000 abstract description 9
- 239000002390 adhesive tape Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 230000000977 initiatory effect Effects 0.000 abstract description 2
- 238000004544 sputter deposition Methods 0.000 description 81
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 23
- 229910052593 corundum Inorganic materials 0.000 description 23
- 229910001845 yogo sapphire Inorganic materials 0.000 description 23
- 239000010408 film Substances 0.000 description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 14
- 238000004506 ultrasonic cleaning Methods 0.000 description 13
- 239000012459 cleaning agent Substances 0.000 description 12
- 239000012535 impurity Substances 0.000 description 10
- 238000000151 deposition Methods 0.000 description 8
- 230000008021 deposition Effects 0.000 description 8
- 238000004880 explosion Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 230000003749 cleanliness Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000005474 detonation Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- VRBFTYUMFJWSJY-UHFFFAOYSA-N 28804-46-8 Chemical compound ClC1CC(C=C2)=CC=C2C(Cl)CC2=CC=C1C=C2 VRBFTYUMFJWSJY-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011185 multilayer composite material Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a Cu/Ti-W/ceramic composite material and a preparation method thereof, belonging to the technical field of initiating explosive devices. According to the preparation method provided by the invention, the ceramic substrate is subjected to ion bombardment, so that the activity of the surface of the ceramic substrate can be effectively improved, and the combination of the metal thin film layer is facilitated; then, the bombarded ceramic substrate is plated with a Ti-W transition layer in advance through one-time magnetron sputtering, so that the bonding force between the metal exploding foil, namely the pure copper layer, and the ceramic substrate can be effectively improved. The experimental result shows that the film-substrate binding force is tested by a multi-time grid-marking method, the cut edge of the Cu/Ti-W/ceramic composite material is completely smooth, and the grid edge does not have any phenomena of peeling, curling and the like; the thin film does not fall off after being adhered for 10 times by the 3M adhesive tape, the binding force of the thin film meets the requirement of preparing the explosive foil by a subsequent photoetching process, the thin film can be normally used under the severe condition, and the binding force of the explosive foil and ceramics is greatly improved.
Description
Technical Field
The invention relates to the technical field of initiating explosive devices, in particular to a Cu/Ti-W/ceramic composite material and a preparation method thereof.
Background
The foil detonator is composed of reflecting plate (substrate), foil of explosion bridge, flying plate, accelerating chamber and low-sensitivity explosive column, and is safe, reliable and simple in structure. The action principle is as follows: applying high-voltage large pulse current at two ends of explosive foil, instantaneously vaporizing and exploding the center of the explosive foil due to its large resistance to generate high-voltage plasma, which pushes the flying plate under the limitation of reflector plate to cut a small flying plate at the center of accelerating chamber and drive the small flying plate to fly in the accelerating chamber at high speed until the small flying plate impacts the explosive column to generate shock wave of pressure P and action time tau, when P is greater than P, the small flying plate can be instantaneously vaporized and exploded to generate high-voltage plasmanThe detonation occurs when the value of τ reaches the detonation threshold value of the explosive. In the whole device, the exploding foil is a medium for energy conversion, converts electric energy into plasma internal energy, is one of key elements, and is mainly made of Cu, Ag, Al and the like. The reflector plate is used for limiting the space of plasma generated by explosion of the explosion box, preventing the dissipation of the plasma generated by the explosion foil, and enabling the plasma generated by the explosion foil to be used for forming and driving the flying plate as much as possible, and the common material is mainly ceramic. However, the bonding force between the metal exploding foil and the reflector made of ceramic material is poor, the metal exploding foil is easy to fall off, the problems of serious energy dissipation and reduced flying piece driving capability during electric explosion can be caused, and the reliability and the safety of the device are finally influenced.
At present, the reliability and the safety of the whole device are improved mainly by improving the structure of the whole device of the exploding foil initiator and controlling the tool size of a component in the prior art, but the problem of low bonding force between the exploding foil and a reflector plate cannot be fundamentally solved. Furthermore, chinese patent publication No. CN104697405A discloses an EFI chip unit, a method for manufacturing the same, and an exploding foil detonating apparatus based on the chip unit, wherein the EFI chip unit includes: ceramic substrate, metal Ti/Cu layer, Parylene C layer, upper electrode Ti/W/Ti/Cu/Au, Schottky diode and Su8 acceleration chamber. Although the EFI chip unit is prepared in a multilayer composite material mode, the composite material has more components and is easy to generate stray current, and the Schottky diode is required to resist the stray current, so that the cost is increased, and the process is complex and is not easy to control.
Therefore, it is urgently needed to provide a preparation method of a Cu/Ti-W/ceramic composite material, which can effectively improve the bonding force between the metal exploding foil and the ceramic substrate, and has the advantages of simple process and easily controlled parameters.
Disclosure of Invention
The invention aims to provide a Cu/Ti-W/ceramic composite material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a Cu/Ti-W/ceramic composite material, which comprises the following steps:
(1) performing ion bombardment on the ceramic substrate to obtain a bombarded ceramic substrate;
(2) performing first magnetron sputtering on the surface of the bombarded ceramic substrate obtained in the step (1) by taking Ti-W alloy as a target material to obtain a Ti-W/ceramic composite material;
(3) and (3) carrying out second magnetron sputtering on the surface of the Ti-W transition layer of the Ti-W/ceramic composite material obtained in the step (2) by taking pure copper as a target material to obtain the Cu/Ti-W/ceramic composite material.
Preferably, the ions bombarded by the ions in the step (1) are argon plasma obtained by ionizing argon gas; the pressure of the argon is 0.01-0.03 Pa.
Preferably, the ion bombardment time in the step (1) is 1-3 min.
Preferably, the power of the first magnetron sputtering in the step (2) is 40-440W, and the time of the first magnetron sputtering is 2-4 s.
Preferably, the atmosphere of the first magnetron sputtering in the step (2) is a vacuum argon-introduced atmosphere; the vacuum degree of the vacuum is less than or equal to 3 multiplied by 10-4Pa; the flow of argon is 60 to100sccm, and the pressure of argon is 0.6-1 Pa.
Preferably, the thickness of the Ti-W transition layer in the Ti-W/ceramic composite material in the step (2) is 5-10 nm.
Preferably, the Ti-W alloy in the step (2) comprises the following components in percentage by mass: 10% of Ti and 90% of W.
Preferably, the power of the second magnetron sputtering in the step (3) is 40-440W, and the time of the second magnetron sputtering is 1-400 min.
Preferably, the thickness of the Cu layer in the Cu/Ti-W/ceramic composite material in the step (3) is 1-10 μm.
The invention also provides the Cu/Ti-W/ceramic composite material prepared by the preparation method in the technical scheme.
The invention provides a preparation method of a Cu/Ti-W/ceramic composite material, which comprises the following steps: performing ion bombardment on the ceramic substrate to obtain a bombarded ceramic substrate; performing first magnetron sputtering on the surface of the bombarded ceramic substrate by taking Ti-W alloy as a target material to obtain a Ti-W/ceramic composite material; and carrying out secondary magnetron sputtering on the surface of the Ti-W transition layer of the Ti-W/ceramic composite material by taking pure copper as a target material to obtain the Cu/Ti-W/ceramic composite material. According to the invention, the ceramic substrate is subjected to ion bombardment, so that the activity of the surface of the ceramic substrate can be effectively improved, and the combination of the metal thin film layer is facilitated; then, the bombarded ceramic substrate is plated with a Ti-W transition layer by magnetron sputtering for the first time, so that the bonding force between the metal exploding foil, namely the pure copper layer, and the ceramic substrate can be effectively improved. The experimental result shows that the film-substrate binding force is tested by a multi-time grid-marking method, the cut edge of the Cu/Ti-W/ceramic composite material is completely smooth, and the grid edge does not have any phenomena of peeling, curling and the like; the thin film does not fall off after being adhered for 10 times by the 3M adhesive tape, the binding force of the thin film meets the requirement of preparing the explosive foil by a subsequent photoetching process, the thin film can be normally used under the severe condition, and the binding force of the explosive foil and ceramics is greatly improved.
The preparation method provided by the invention is simple and feasible, the parameters are easy to control, the cost is low, and the large-scale production can be realized.
Drawings
FIG. 1 is a microstructure diagram of a copper metal film observed by an atomic force microscope of a Cu/Ti-W/ceramic composite material prepared in example 1 of the present invention;
FIG. 2 is a microstructure diagram of a copper metal film observed by an atomic force microscope of a Cu/Ti-W/ceramic composite material prepared in example 2 of the present invention;
FIG. 3 is a diagram of an actual surface state of the Cu/Ti-W/ceramic composite material prepared in example 1 of the present invention after a cross-hatch test.
Detailed Description
The invention provides a preparation method of a Cu/Ti-W/ceramic composite material, which comprises the following steps:
(1) performing ion bombardment on the ceramic substrate to obtain a bombarded ceramic substrate;
(2) performing first magnetron sputtering on the surface of the bombarded ceramic substrate obtained in the step (1) by taking Ti-W alloy as a target material to obtain a Ti-W/ceramic composite material;
(3) and (3) carrying out second magnetron sputtering on the surface of the Ti-W transition layer of the Ti-W/ceramic composite material obtained in the step (2) by taking pure copper as a target material to obtain the Cu/Ti-W/ceramic composite material.
The method carries out ion bombardment on the ceramic substrate to obtain the bombarded ceramic substrate.
In the invention, the ceramic substrate is preferably cleaned before ion bombardment; the cleaning treatment comprises the steps of sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents to carry out ultrasonic cleaning respectively; the total time of the cleaning treatment is preferably 20-30 min. According to the invention, impurities on the surface of the ceramic substrate can be effectively removed by cleaning the ceramic substrate, and the bonding force with the metal exploding foil, namely a Cu layer, is improved.
In the present invention, the material of the ceramic substrate is preferably Al2O3。
In the invention, the ions bombarded by the ions are preferably argon plasma obtained by ionizing argon gas; the pressure of the argon is preferably 0.01-0.03 Pa, and more preferably 0.02 Pa. According to the invention, the argon plasma obtained by ionizing argon is adopted for ion bombardment, and the pressure of the argon is controlled within the range, so that the surface of the ceramic substrate has higher activity and cleanliness, and the bonding force between the ceramic substrate and the metal exploding foil, namely the Cu layer, can be improved.
In the invention, the time of the ion bombardment is preferably 1-3 min, and more preferably 2 min. The invention can make the activity and the cleanness of the ceramic substrate higher by controlling the ion bombardment time in the range.
After the bombarded ceramic substrate is obtained, the Ti-W alloy is used as a target material, and the first magnetron sputtering is carried out on the surface of the bombarded ceramic substrate to obtain the Ti-W/ceramic composite material.
In the present invention, the Ti — W alloy preferably includes the following components in percentage by mass: 10% of Ti and 90% of W. According to the invention, by selecting the Ti-W alloy with the components, the Ti-W transition layer can be formed on the surface of the bombarded ceramic substrate in advance, and the Ti-W transition layer is ensured to be firmly combined with the surface of the bombarded ceramic substrate, and meanwhile, a stable and firmly combined interface can be formed with the Cu layer, so that the bonding force between metal, namely the Cu layer and the ceramic substrate is effectively improved.
In the present invention, the Ti — W alloy is preferably pre-sputtered prior to use. The invention has no special requirements on the power and time of the pre-sputtering, and can adopt sputtering parameters which are well known to those skilled in the art. According to the invention, by pre-sputtering before use, oxidized metal and other impurities on the surface of the Ti-W alloy can be removed, the cleanliness of the Ti-W transition layer is improved, and the bonding force between the metal exploding foil and the ceramic matrix is more favorably realized.
In the invention, the bombarded ceramic substrate is preferably kept at a constant temperature in the integral preparation process; the constant temperature is preferably room temperature to 320 ℃, more preferably 100 to 300 ℃, and most preferably 150 to 250 ℃. The invention is more beneficial to improving the bonding force between the metal exploding foil and the ceramic substrate by controlling the temperature of the bombarded ceramic substrate within the range.
In the invention, the power of the first magnetron sputtering is preferably 40-440W, more preferably 80-400W, and most preferably 100-350W; the time of the first magnetron sputtering is preferably 2-4 s, and more preferably 2-3 s. By controlling the power and time of the first magnetron sputtering within the range, the method can ensure that the sputtered Ti and W have higher deposition rate and impact the surface of the ceramic substrate at high speed, and is more favorable for obtaining a uniform and smooth Ti-W transition layer which is firmly combined with the surface of the ceramic substrate.
In the invention, the atmosphere of the first magnetron sputtering is preferably an atmosphere of vacuum argon introduction; the vacuum degree of the vacuum is preferably less than or equal to 3 x 10-4Pa; the flow rate of the argon gas is preferably 60-100 sccm, more preferably 70-90 sccm, and most preferably 80 sccm; the pressure of the argon gas is preferably 0.6-1 Pa, more preferably 0.7-0.9 Pa, and most preferably 0.8 Pa. According to the invention, the atmosphere, the vacuum degree, the argon flow and the argon pressure of the first magnetron sputtering are controlled to be in the above ranges, so that the contact between sputtered particles and air can be avoided, the argon has higher ionization rate, and the argon plasma obtained by ionization bombards the target at high speed, so that the target particles moving at high speed are obtained and impact on the surface of the substrate at high speed, and the firm combination is realized.
In the invention, the thickness of the Ti-W transition layer in the Ti-W/ceramic composite material is preferably 5-10 nm, more preferably 6-9 nm, and most preferably 7-8 nm. According to the invention, the Ti-W transition layer which is flat, uniform and strong in binding force with the ceramic matrix is more favorably obtained by controlling the thickness of the Ti-W transition layer within the range, so that the binding force between the metal explosion foil and the ceramic matrix is effectively improved.
After the Ti-W/ceramic composite material is obtained, the Cu/Ti-W/ceramic composite material is obtained by performing secondary magnetron sputtering on the surface of the Ti-W transition layer of the Ti-W/ceramic composite material by taking pure copper as a target material.
In the present invention, the purity of the pure copper is preferably > 99.99%.
In the invention, the temperature of the Ti-W/ceramic composite material is preferably room temperature to 320 ℃, more preferably 100 to 300 ℃, and most preferably 150 to 250 ℃. According to the invention, the temperature of the Ti-W/ceramic composite material is controlled within the range, so that the bonding force between the Ti-W/ceramic composite material and the Cu layer is improved, and the high bonding force between the metal explosion foil and the ceramic substrate is ensured.
In the present invention, the pure copper is preferably pre-sputtered prior to use. The invention has no special requirements on the power and time of the pre-sputtering, and can adopt sputtering parameters which are well known to those skilled in the art. The invention can remove the oxidized metal and other impurities on the surface of the pure copper target material by pre-sputtering before use, improves the cleanliness of the pure copper target material and is more beneficial to realizing the binding force between the metal exploding foil and the ceramic matrix.
In the invention, the power of the second magnetron sputtering is preferably 40-440W, more preferably 100-400W, and most preferably 200-300W; the time of the second magnetron sputtering is preferably 1-400 min, more preferably 10-350 min, and most preferably 50-300 min. According to the invention, the power and time of the second magnetron sputtering are controlled within the range, so that the sputtered Cu has a high deposition rate and can impact the surface of the Ti-W transition layer at a high speed, and a uniform, flat and firmly combined Cu layer of the Ti-W transition layer can be obtained.
In the invention, the thickness of the Cu layer in the Cu/Ti-W/ceramic composite material is preferably 1-10 μm, more preferably 2-8 μm, and most preferably 4-6 μm. According to the invention, the thickness of the Cu layer is controlled within the range, so that the Cu layer obtained by sputtering is more uniform and flat, and has higher binding force with the Ti-W/ceramic composite material.
The Cu/Ti-W/ceramic composite material prepared by the preparation method provided by the invention has no peeling, curling and other phenomena among layers; the film does not fall off after being adhered for 10 times by the 3M adhesive tape, and the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the film can still be normally used under the severe condition; the preparation method provided by the invention is simple and feasible, the parameters are easy to control, the cost is low, and the large-scale production can be realized.
The invention also provides the Cu/Ti-W/ceramic composite material prepared by the preparation method in the technical scheme.
The Cu layer in the Cu/Ti-W/ceramic composite material provided by the invention is firmly combined with the matrix, and the reliability and safety of the whole device can be ensured when the Cu/Ti-W/ceramic composite material is used as an element of an exploding foil initiator.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the cleaning agents in an ultrasonic cleaning machine for ultrasonic cleaning and cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; wherein, the ion of ion bombardment is argon plasma obtained by ionizing argon, and the pressure of the argon is 0.02 Pa.
(2) Mounting the target material and Al2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was room temperature. Pre-sputtering Ti-W alloy target for 10min and pure copper target for 10min to remove impurities on the surface of the target, wherein Al is the impurity2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the sputtering is finished.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the condition of the atmosphere parameters, the first sputtering power is set to be 120W, the first sputtering time is 2s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 7.5 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is room temperature, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 40min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 3.5 mu m.
The microstructure of the copper metal thin film observed by observing the Cu/Ti-W/ceramic composite material prepared in example 1 by using an atomic force microscope is shown in FIG. 1. As can be seen from FIG. 1, the film surface is continuous and the surface roughness is low (note: the height of 52nm in FIG. 1 is not the actual thickness of the Cu layer film, but the height of the surface relief of the microstructure).
Test 1
The Cu/Ti-W/ceramic composite material prepared in example 1 was subjected to a multi-pass lattice test for film-substrate bonding force, and the test results are shown in fig. 3. As can be seen from FIG. 3, the cut edge is completely smooth, the grid edge does not have any phenomena of peeling, curling and the like, and the bonding force of the cut edge meets the requirement of preparing the exploding foil by the subsequent photoetching process, and the exploding foil can be normally used under the conventional condition.
Example 2
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the cleaning agents in an ultrasonic cleaning machine for ultrasonic cleaning and cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; wherein, the ion of ion bombardment is argon plasma obtained by ionizing argon, and the pressure of the argon is 0.02 Pa.
(2) Mounting the target material and Al2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was 150 ℃. The Ti-W alloy target material is pre-sputtered for 10min and the pure copper target material is pre-sputtered for the same 10minRemoving impurities on the surface of the target material, wherein Al is2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the sputtering is finished.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the condition of the atmosphere parameters, the first sputtering power is set to be 120W, the first sputtering time is 2s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 7.5 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is 150 ℃, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 40min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 3.5 mu m.
The Cu/Ti-W/ceramic composite material prepared in example 2 was observed by an atomic force microscope, and the microstructure of the observed Cu metal thin film is shown in FIG. 2. As can be seen from FIG. 2, the film surface is continuous, and the roughness is increased compared with example 1, but the grooves and holes are obviously reduced, and the film quality is greatly improved (note: the height of 0.23 μm in FIG. 1 is not the actual thickness of the Cu layer film, but the height of the surface relief of the microstructure).
Test 2
The Cu/Ti-W/ceramic composite material prepared in the embodiment 2 is adhered for 10 times by a 3M adhesive tape, a film does not fall off, the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the explosive foil can be normally used under a severe condition.
Example 3
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the cleaning agents in an ultrasonic cleaning machine for ultrasonic cleaning and cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; therein, get awayThe ion bombarded by the ion is argon plasma obtained by ionizing argon, and the pressure of the argon is 0.02 Pa.
(2) The target material and Al are well installed2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was 150 ℃. Carrying out pre-sputtering on the Ti-W alloy target for 10min and carrying out the same pre-sputtering on the pure copper target for 10min to remove impurities on the surface of the target, wherein Al is at the moment2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the sputtering is finished.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the condition of the atmosphere parameters, the first sputtering power is set to be 120W, the first sputtering time is 2.5s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 8.5 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is 200 ℃, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 53min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 4.2 mu m.
The Cu/Ti-W/ceramic composite material prepared in the embodiment 3 is adhered for 10 times by a 3M adhesive tape, a film does not fall off, the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the explosive foil can be normally used under a severe condition.
Example 4
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the ceramic substrate in an ultrasonic cleaning machine for ultrasonic cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; wherein the ion bombarded ion is argonThe argon plasma obtained by ionization has the argon pressure of 0.02 Pa.
(2) Mounting the target material and Al2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was 150 ℃. Carrying out pre-sputtering on the Ti-W alloy target for 10min and carrying out the same pre-sputtering on the pure copper target for 10min to remove impurities on the surface of the target, wherein Al is at the moment2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the sputtering is finished.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the condition of the atmosphere parameters, the first sputtering power is set to be 120W, the first sputtering time is 3s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 9.3 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is 220 ℃, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 60min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 4.6 mu m.
The Cu/Ti-W/ceramic composite material prepared in the embodiment 4 is adhered for 10 times by a 3M adhesive tape, a film does not fall off, the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the explosive foil can be normally used under a severe condition.
Example 5
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the cleaning agents in an ultrasonic cleaning machine for ultrasonic cleaning and cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; wherein the ion bombarded by the ion is argon plasma obtained by ionizing argonThe pressure of argon is 0.02 Pa.
(2) The target material and Al are well installed2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was 150 ℃. Carrying out pre-sputtering on the Ti-W alloy target for 10min and carrying out the same pre-sputtering on the pure copper target for 10min to remove impurities on the surface of the target, wherein Al is at the moment2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the target material is completely sputtered.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the atmosphere parameter condition, the first sputtering power is set to be 120W, the first sputtering time is 3s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 9.3 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is 220 ℃, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 70min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 5 mu m.
The Cu/Ti-W/ceramic composite material prepared in the embodiment 5 is adhered for 10 times by a 3M adhesive tape, a film does not fall off, the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the explosive foil can be normally used under a severe condition.
Example 6
The preparation method of the Cu/Ti-W/ceramic composite material provided by the embodiment specifically comprises the following steps:
(1) mixing Al2O3Sequentially adopting acetone, deionized water and absolute ethyl alcohol as cleaning agents for the ceramic substrate, placing the cleaning agents in an ultrasonic cleaning machine for ultrasonic cleaning and cleaning for 20min, drying, and then cleaning the cleaned Al2O3Performing ion bombardment on the ceramic substrate for 2 min; wherein, the ion of ion bombardment is argon plasma obtained by ionizing argon, and the pressure of the argon is 0.02 Pa.
(2) Mounting the target material and Al2O3Vacuumizing the ceramic substrate until the vacuum degree is lower than 3 x 10-4Introducing argon after Pa, adjusting the pressure of the argon to be 0.8Pa, the flow of the argon to be 80sccm and Al2O3The ceramic substrate temperature was 150 ℃. Carrying out pre-sputtering on the Ti-W alloy target for 10min and carrying out the same pre-sputtering on the pure copper target for 10min to remove impurities on the surface of the target, wherein Al is at the moment2O3The ceramic substrate is not opposite to the target material, and the sputtering power supply is turned off after the sputtering is finished.
After the pre-sputtering is finished, the Ti-W alloy target material and Al are mixed2O3And (3) the ceramic substrate is opposite, a sputtering power supply is turned on under the condition of the atmosphere parameters, the first sputtering power is set to be 120W, the first sputtering time is 3.5s, and the Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Ti-W transition layer is 10 nm.
(3) And after the deposition of the transition layer is finished, the pure copper target is opposite to one surface of the Ti-W transition layer of the Ti-W/ceramic composite material, under the condition of the atmosphere parameters, the temperature of the Ti-W/ceramic composite material is 260 ℃, a sputtering power supply is turned on, the second sputtering power is set to be 120W, the second sputtering time is 80min, and the Cu/Ti-W/ceramic composite material is obtained after the sputtering is finished, wherein the thickness of the Cu layer is 6 mu m.
The Cu/Ti-W/ceramic composite material prepared in the embodiment 6 is adhered for 10 times by a 3M adhesive tape, a film does not fall off, the binding force of the film meets the requirement of preparing an explosive foil by a subsequent photoetching process, and the explosive foil can be normally used under a severe condition.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a Cu/Ti-W/ceramic composite material comprises the following steps:
(1) performing ion bombardment on the ceramic substrate to obtain a bombarded ceramic substrate;
(2) performing first magnetron sputtering on the surface of the bombarded ceramic substrate obtained in the step (1) by taking Ti-W alloy as a target material to obtain a Ti-W/ceramic composite material;
(3) and (3) carrying out second magnetron sputtering on the surface of the Ti-W transition layer of the Ti-W/ceramic composite material obtained in the step (2) by taking pure copper as a target material to obtain the Cu/Ti-W/ceramic composite material.
2. The method according to claim 1, wherein the ions to be ion-bombarded in the step (1) are argon plasma obtained by ionizing argon gas; the pressure of the argon is 0.01-0.03 Pa.
3. The method according to claim 1 or 2, wherein the ion bombardment time in the step (1) is 1-3 min.
4. The preparation method of claim 1, wherein the power of the first magnetron sputtering in the step (2) is 40-440W, and the time of the first magnetron sputtering is 2-4 s.
5. The method according to claim 1 or 4, wherein the atmosphere of the first magnetron sputtering in the step (2) is a vacuum argon-filled atmosphere; the vacuum degree of the vacuum is less than or equal to 3 multiplied by 10-4Pa; the flow of the argon is 60-100 sccm, and the pressure of the argon is 0.6-1 Pa.
6. The method according to claim 1, wherein the thickness of the Ti-W transition layer in the Ti-W/ceramic composite material in the step (2) is 5 to 10 nm.
7. The preparation method of claim 1, wherein the Ti-W alloy in the step (2) comprises the following components in percentage by mass: 10% of Ti and 90% of W.
8. The preparation method of claim 1, wherein the power of the second magnetron sputtering in the step (3) is 40-440W, and the time of the second magnetron sputtering is 1-400 min.
9. The method according to claim 1, wherein the thickness of the Cu layer in the Cu/Ti-W/ceramic composite material in the step (3) is 1 to 10 μm.
10. A Cu/Ti-W/ceramic composite material prepared by the preparation method of any claim 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210349511.9A CN114540754A (en) | 2022-04-02 | 2022-04-02 | Cu/Ti-W/ceramic composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210349511.9A CN114540754A (en) | 2022-04-02 | 2022-04-02 | Cu/Ti-W/ceramic composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114540754A true CN114540754A (en) | 2022-05-27 |
Family
ID=81664931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210349511.9A Pending CN114540754A (en) | 2022-04-02 | 2022-04-02 | Cu/Ti-W/ceramic composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114540754A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992017622A1 (en) * | 1991-04-08 | 1992-10-15 | Tosoh Smd, Inc. | Thermally compatible sputter target and backing plate assembly |
| TW200924877A (en) * | 2007-07-18 | 2009-06-16 | Sanyo Special Steel Co Ltd | Method for producing sputtering target material for Ni-W based interlayer |
| CN110195209A (en) * | 2019-06-12 | 2019-09-03 | 西南科技大学 | Outer broadband light absorbing material of a kind of visible red and preparation method thereof |
| CN111721163A (en) * | 2019-03-18 | 2020-09-29 | 南京理工大学 | Microchip integrated exploding foil initiator based on plane high-voltage switch |
-
2022
- 2022-04-02 CN CN202210349511.9A patent/CN114540754A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992017622A1 (en) * | 1991-04-08 | 1992-10-15 | Tosoh Smd, Inc. | Thermally compatible sputter target and backing plate assembly |
| TW200924877A (en) * | 2007-07-18 | 2009-06-16 | Sanyo Special Steel Co Ltd | Method for producing sputtering target material for Ni-W based interlayer |
| CN111721163A (en) * | 2019-03-18 | 2020-09-29 | 南京理工大学 | Microchip integrated exploding foil initiator based on plane high-voltage switch |
| CN110195209A (en) * | 2019-06-12 | 2019-09-03 | 西南科技大学 | Outer broadband light absorbing material of a kind of visible red and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 周全: "铜***箔制备工艺对微结构及电爆一致性的影响研究", no. 01, pages 017 - 89 * |
| 赵时璐: "《多弧离子镀Ti-Al-Zr-Cr-N系复合硬质膜》", vol. 1, 冶金工业出版社, pages: 105 - 106 * |
| 黄娜等: "冲击片******箔的制备与电爆性能", vol. 22, no. 4, pages 514 - 520 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3945902A (en) | Metallized device and method of fabrication | |
| CN109518148B (en) | Method for preparing vanadium dioxide intelligent thermal control device by high-energy pulse reaction magnetron sputtering | |
| CN109297364A (en) | A kind of microchip Exploding foil initiator and preparation method thereof containing Al/PTFE | |
| CN114540754A (en) | Cu/Ti-W/ceramic composite material and preparation method thereof | |
| CN109440074B (en) | High-energy-output hydrogen explosion membrane bridge and preparation method thereof | |
| JPS5864017A (en) | Ceramic condenser and method of producing same | |
| US11299801B2 (en) | Structure and method to fabricate highly reactive physical vapor deposition target | |
| CN106319468A (en) | Method for increasing quality of magnetron sputtering coating | |
| CN111607771A (en) | Atomic oxygen resistant polymer film material and preparation method thereof | |
| TWI810631B (en) | Method for forming metallic nano-twinned thin film structure | |
| CN115028477A (en) | DSC ceramic metallization technology and ceramic packaging substrate prepared by same | |
| CN109612342A (en) | Microchip Exploding foil initiator and preparation method thereof based on bridge foil in parallel | |
| RU2645438C1 (en) | Method of making photoconverter with built-in diode | |
| JP2002111176A (en) | Method of forming conduction path and substrate | |
| CN109680254B (en) | Magnesium-aluminum alloy hydrogen-carrying thin film material and preparation method thereof | |
| TW202314006A (en) | Nano-twinned structure on metallic thin film surface and method for forming the same | |
| CN110923636B (en) | Electron beam composite plasma alloying treatment method for surface of gamma-TiAl alloy | |
| WO2017020535A1 (en) | Copper/aluminium alloy crystal oscillation plate coating process | |
| CN115732321A (en) | Wafer etching and cleaning equipment and method | |
| JP2986948B2 (en) | AlN circuit board | |
| RU2069915C1 (en) | Process of manufacture of secondary emission cathode | |
| CN112030117B (en) | Method for preparing aluminum oxide coating by modulating high-current pulse arc | |
| JPH01195272A (en) | Sputtering device | |
| CN116136380A (en) | Impact piece transduction element based on Ti/Al ablation layer and preparation method thereof | |
| JPH11298122A (en) | Circuit board and manufacture thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220527 |
|
| RJ01 | Rejection of invention patent application after publication |