CN112786772B - Infrared enhanced absorption metal nano material and preparation method thereof - Google Patents

Infrared enhanced absorption metal nano material and preparation method thereof Download PDF

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CN112786772B
CN112786772B CN202110026188.7A CN202110026188A CN112786772B CN 112786772 B CN112786772 B CN 112786772B CN 202110026188 A CN202110026188 A CN 202110026188A CN 112786772 B CN112786772 B CN 112786772B
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lithium tantalate
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CN112786772A (en
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明安杰
赵永敏
朱婧
张少勋
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GRIMN Engineering Technology Research Institute Co Ltd
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    • 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
    • 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
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    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract

An infrared enhanced absorption metal nano material and a preparation method thereof, wherein the material comprises the following components: the lower surface of the lithium tantalate wafer is sequentially provided with a Ti/Cr layer and an Au layer from top to bottom, and the upper surface of the lithium tantalate wafer is sequentially provided with a Ti/Cr layer, an Al layer and a gold black layer from bottom to top. The method comprises the following steps: sequentially preparing a Ti/Cr layer and an Au layer from top to bottom on the lower surface of the lithium tantalate wafer, and sequentially preparing the Ti/Cr layer and an Al layer from bottom to top on the upper surface of the lithium tantalate wafer; preparing a high polymer adhesion layer on the surface of the Al layer; placing a stainless steel mask plate above the lithium tantalate wafer; the gold black layer is prepared on the upper surface of the polymer adhesive layer by adopting high-purity gold particles as raw materials and adopting a thermal evaporation mode in an inert gas atmosphere. The method has the advantages of improving the wide spectrum absorptivity, improving the substrate adhesiveness and realizing the large-area preparation of the patterns, along with simple preparation process, good product reliability and suitability for industrial production.

Description

Infrared enhanced absorption metal nano material and preparation method thereof
Technical Field
The invention relates to the field of infrared sensor functional materials, in particular to an infrared enhanced absorption metal nano material and a preparation method thereof.
Background
The infrared detector and the module system have important military and commercial application values. Infrared detectors are currently used in many industries such as internet of things intelligent hardware, NDIR gas sensors, security alarm systems, carbon sulfur instruments, flame detection modules, and the like. Uncooled infrared detectors based on pyroelectric and thermopile principles are increasingly used in the infrared detection field due to the advantages of short response time, low noise, wide detection band, no need of refrigeration and the like.
The performance of the pyroelectric infrared detector is mainly characterized by the detection rate, response time and the like, and the performance of the infrared absorption material is closely related to the performance of the detector. To obtain a higher detection rate in the mid-infrared broadband range, the absorption rate of the absorption layer of the detector to infrared rays is required to be high (i.e., the reflectivity is low); a fast response speed requires a small heat capacity of the absorption layer. Therefore, the infrared absorption functional layer with higher absorptivity in a broad-spectrum and broad-band range is critical to the performance of the pyroelectric detector, and the core parameter indexes such as response time, detection rate and the like are directly influenced.
In recent years, research on infrared reinforced absorbing materials by various scientific research teams and companies at home and abroad has achieved a certain result, and the most main absorbing layer materials are classified into the following categories: (1) the nano carbon material has good nano structure and higher absorptivity, but has narrow absorption bandwidth, can only face common gas detection, has poor adhesion with a substrate and is easy to fall off, and in addition, the preparation process of the high absorptivity carbon nano tube is complex, the graphene is difficult to transfer, and the preparation process is not compatible with the development of actual products; (2) the metamaterial can realize complete absorption of light by designing structural parameters, but has the same problems as the metamaterial and carbon black, namely, the metamaterial has a narrow absorption bandwidth and can be only used as an infrared absorption layer of an infrared detector facing common gas detection; (3) the NiCr alloy absorbing material has high requirement on magnetron sputtering equipment by substrate rotation in the preparation process; (4) the porous gold black absorbing material has the absorptivity of the gold black infrared absorbing layer prepared by adopting thermal evaporation over 95%, can realize wide-spectrum detection, and can reach the best compromise between high absorptivity and low heat capacity, but has the problems in application: the gold-black film has a brittle structure, poor adhesion with a substrate, easy falling off in practical application, and compatibility with wafer-level patterning preparation is still to be further developed, so that the application of the gold-black film is limited to a certain extent.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the infrared enhanced absorption metal nano material which has high absorption in a middle infrared band and a wide spectrum range, good adhesion and can be patterned at a wafer level and the preparation method thereof.
The invention is realized by the following technical scheme.
An infrared enhanced absorption metal nanomaterial, the material comprising: the lithium tantalate wafer, the lower surface of lithium tantalate wafer is equipped with Ti/Cr layer (namely Ti layer or Cr layer) and Au layer in proper order from top to bottom, the upper surface of lithium tantalate wafer is equipped with Ti/Cr layer and Al layer, polymer adhesion layer and gold black layer from bottom to top in proper order.
Further, the polymer adhesive layer is 502 glue or AB glue.
The preparation method of the infrared enhanced absorption metal nano material is characterized by comprising the following steps of:
(1) Sequentially preparing a Ti/Cr layer and an Au layer from top to bottom on the lower surface of the lithium tantalate wafer, and sequentially preparing the Ti/Cr layer and an Al layer from bottom to top on the upper surface of the lithium tantalate wafer;
(2) Preparing a high polymer adhesion layer on the surface of the Al layer;
(3) Placing a stainless steel mask plate above the lithium tantalate wafer obtained in the step (2);
(4) The gold black layer is prepared on the upper surface of the polymer adhesive layer by adopting high-purity gold particles as raw materials and adopting a thermal evaporation mode in an inert gas atmosphere.
Further, the preparation method adopted in the step (1) is a magnetron sputtering or thermal evaporation method.
Further, the thickness of the Ti/Cr layer in the step (1) is 1-20 nm, the thickness of the Au layer is 100-500 nm, and the thickness of the Al layer is 200-800 nm.
Further, the polymer adhesive layer in the step (2) is 502 glue or AB glue (a double-component epoxy resin AB glue adhesive), and the preparation method is fumigation or spin coating of the fumigation display cabinet.
Further, the step (4) is performed with thermal evaporation in a nitrogen atmosphere: placing high-purity gold (99.999%) raw material into molybdenum boat or tungsten boat, adjusting the distance between lithium tantalate wafer and molybdenum boat or tungsten boat to 1-10cm, extracting vacuum degree to below 1Pa, and keeping introducing N 2 Regulating N for 5-10min 2 The air pressure is 1500Pa-4000Pand a, regulating the current to 10A-200A, and evaporating gold particles in the molybdenum boat or the tungsten boat until no gold material remains, thereby obtaining a gold black layer.
Further, the thickness of the gold black layer is 200 nm-5 um.
The beneficial technical effects of the invention are as follows:
1. according to the invention, through the introduction of the high polymer adhesive layer, the adhesion between the gold-black film material and the substrate (lithium carbonate wafer) is improved, so that the mechanical reliability of the gold-black film material in practical application is ensured.
2. The invention realizes the wafer-level graphical preparation by introducing the stainless steel hard mask, and meets the actual production requirement.
3. The infrared absorption rate of the gold-black film material is closely related to the preparation process, and the gold-black film material with further improved infrared absorption rate can be obtained by adjusting the evaporation capacity, the air pressure, the current and the distance between the substrate and the boat.
4. The method can further improve the wide-spectrum absorptivity, improve the substrate adhesiveness and realize the large-area preparation of the patterns, and is simple in preparation process, good in product reliability and suitable for industrial production.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a low magnification SEM image of the microscopic morphology of the gold black thin film material.
Fig. 3 is a high magnification SEM image of the microscopic morphology of the gold black thin film material.
Fig. 4 is a fourier infrared spectrum test absorbance spectrum of a gold black thin film material.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
An infrared enhanced absorption metal nanomaterial comprising: the lower surface of the lithium tantalate wafer is sequentially provided with a Ti/Cr layer and an Au layer from top to bottom, and the upper surface of the lithium tantalate wafer is sequentially provided with a Ti/Cr layer, an Al layer, a high polymer adhesion layer and a gold black layer (namely a black gold layer from bottom to top).
Example 1
The specific process steps for preparing the infrared enhanced absorption metal nano material are as follows:
(1) Firstly, cleaning a lithium tantalate wafer by using acetone, alcohol and deionized water, then sequentially preparing a transition layer Ti layer and a top electrode Al layer on the upper surface of the lithium tantalate wafer by using a magnetron sputtering method, and sequentially preparing a transition layer Ti layer and a bottom electrode Au layer on the lower surface of the lithium tantalate wafer. Wherein, the argon flow is controlled to be 20sccm, the argon pressure is controlled to be 0.5Pa, the power of a direct current power supply is 50W, the thickness of the prepared Ti layer is 20nm, the thickness of the top electrode Al layer is 500nm, and the thickness of the bottom electrode Au layer is 300nm.
(2) Fumigating the surface of the Al layer of the top electrode by using 502 glue with a fumigating cabinet, injecting 5g of 502 glue into a container, and then adding 15mL of water into the container on the water heater. Heating for 20min, fumigation for 20min, and exhausting for 15min. An adhesion layer is obtained 502.
(3) And (3) adopting a stainless steel mask plate, designing a pattern of an absorption material on the surface of the sensitive element, leaving a subsequent detector preparation wiring position, and placing the mask plate above the lithium tantalate wafer to fix the relative position of the mask plate.
(4) The thermal evaporation equipment is nitrogen gas circuit equipment, 0.2g of gold particles (purity is 99.999%) are placed in a molybdenum boat, the distance between a substrate (lithium tantalate wafer) and the boat is regulated to 6cm, a mechanical pump and a bypass valve are opened, the vacuum degree is extracted to be less than 1Pa, and N is opened 2 Gas circuit valve for regulating N 2 The air pressure is kept at 3000Pa for 5min, and redundant oxygen is removed. And starting the substrate to rotate, regulating the evaporation current to 170A, enabling gold particles in the evaporation boat to be free of residues, turning off a heating power supply, and cooling the equipment along with the furnace for 30min to obtain the wafer-level patterned gold-black film layer metal nano material with good adhesion effect and thickness of 1 um.
The infrared enhanced absorption metal nano material with the gold-black film layer obtained by the embodiment is subjected to microstructure observation to obtain a scanning electron microscope photo, and the scanning electron microscope photo is shown as a picture 2 and a picture 3, so that the structure is loose and porous, the uniformity is good, gold particles are stacked in a spherical shape, and attenuation is caused by repeated reflection of infrared light, so that the infrared broad spectrum absorption effect is realized. Fig. 4 shows that the infrared enhanced absorption metal nanomaterial with gold-black thin film layer obtained in this embodiment has an absorption rate of more than 98% in the wavelength band of 2.5um-20 um.
Example 2
(1) Firstly, cleaning a lithium tantalate wafer by using acetone, alcohol and deionized water, then sequentially preparing a transition layer Ti layer and a top electrode Al layer on the upper surface of the lithium tantalate wafer by using a magnetron sputtering method, and sequentially preparing a transition layer Ti layer and a bottom electrode Au layer on the lower surface of the lithium tantalate wafer. Wherein, the argon flow is 20sccm, the argon pressure is 0.5Pa, the direct current power is 50W, the thickness of the prepared Ti layer is 20nm, the thickness of the top electrode Al layer is 500nm, and the thickness of the bottom electrode Au layer is 300nm.
(2) And (3) spin coating 502 glue by adopting a spin coater, firstly, adsorbing an Al layer of a top electrode of the lithium tantalate wafer on the spin coater upwards, then, dripping 5g of 502 glue on the surface of the electrode, and spin coating at 600rpm for 10s and 3000rpm for 30s to obtain a 502 adhesive layer.
(3) And (3) adopting a stainless steel mask plate, designing a pattern of an absorption material on the surface of the sensitive element, leaving a subsequent detector preparation wiring position, and placing the mask plate above the lithium tantalate wafer to fix the relative position of the mask plate.
(4) The thermal evaporation equipment is nitrogen gas path equipment, 0.1g of gold particles are placed in a molybdenum boat, the distance between a substrate and the boat is regulated to 7cm, a mechanical pump and a bypass valve are opened, the vacuum degree is extracted to be less than 1Pa, and N is opened 2 Gas circuit valve for regulating N 2 The air pressure is up to 4000Pa and kept for 5min, and redundant oxygen is removed. And starting the substrate to rotate, regulating the evaporation current to 170A, enabling gold particles in the evaporation boat to be free of residues, turning off a heating power supply, and cooling the equipment along with the furnace for 30min to obtain the infrared enhanced absorption metal nano material with the wafer-level graphical gold-black film layer thickness of 500nm and good adhesion effect.
Example 3
(1) Firstly, cleaning a lithium tantalate wafer by using acetone, alcohol and deionized water, sequentially preparing a transition layer Cr layer and a top electrode Al layer on the upper surface of the lithium tantalate wafer by a thermal evaporation method, and sequentially preparing a transition layer Cr layer and a bottom electrode Au layer on the lower surface of the lithium tantalate wafer. Wherein, the argon flow is 20sccm, the argon pressure is 0.5Pa, the direct current power is 50W, the thickness of the prepared Cr layer is 5nm, the thickness of the top electrode Al layer is 800nm, and the thickness of the bottom electrode Au layer is 100nm.
(2) And spin-coating the AB glue by adopting a spin-coating machine, firstly, adsorbing an Al layer of a top electrode of the lithium tantalate wafer on the spin-coating machine upwards, then, dripping 5g of the AB glue on the surface of the electrode, spin-coating at 600rpm for 10s, and spin-coating at 3000rpm for 30s to obtain an AB glue adhesive layer.
(3) And (3) adopting a stainless steel mask plate, designing a pattern of an absorption material on the surface of the sensitive element, leaving a subsequent detector preparation wiring position, and placing the mask plate above the lithium tantalate wafer to fix the relative position of the mask plate.
(4) The thermal evaporation equipment is nitrogen gas path equipment, 1g of gold particles are placed in a tungsten boat, the distance between a substrate and the boat is adjusted to be 10cm, a mechanical pump and a bypass valve are opened, the vacuum degree is extracted to be less than 1Pa, and N is opened 2 Gas circuit valve for regulating N 2 The air pressure is kept at 1500Pa for 10min, and redundant oxygen is removed. And (3) starting the substrate to rotate, regulating the evaporation current to 20A, enabling gold particles in the evaporation boat to be free of residues, turning off a heating power supply, and cooling the equipment along with a furnace for 30min to obtain the wafer-level imaging infrared enhanced absorption metal nano material with good adhesion effect, wherein the thickness of the gold-black film layer is 5um.
Example 4
(1) Firstly, cleaning a lithium tantalate wafer by using acetone, alcohol and deionized water, sequentially preparing a transition layer Cr layer and a top electrode Al layer on the upper surface of the lithium tantalate wafer by a thermal evaporation method, and sequentially preparing a transition layer Cr layer and a bottom electrode Au layer on the lower surface of the lithium tantalate wafer. Wherein, the argon flow is 20sccm, the argon pressure is 0.5Pa, the direct current power is 50W, the thickness of the prepared Cr layer is 10nm, the thickness of the top electrode Al layer is 200nm, and the thickness of the bottom electrode Au layer is 500nm.
(2) And (3) spin coating 502 glue by adopting a spin coater, firstly, adsorbing an Al layer of a top electrode of the lithium tantalate wafer on the spin coater upwards, then, dripping 5g of 502 glue on the surface of the electrode, and spin coating at 600rpm for 10s and 3000rpm for 30s to obtain a 502 glue adhesive layer.
(3) And (3) adopting a stainless steel mask plate, designing a pattern of an absorption material on the surface of the sensitive element, leaving a subsequent detector preparation wiring position, and placing the mask plate above the lithium tantalate wafer to fix the relative position of the mask plate.
(4) The thermal evaporation equipment is nitrogen gas path equipment, 0.6g of gold particles are placed in a tungsten boat, the distance between a substrate and the boat is regulated to be 3cm, a mechanical pump and a bypass valve are opened, the vacuum degree is extracted to be less than 1Pa, and N is opened 2 Gas circuit valve for regulating N 2 The air pressure is kept at 2000Pa for 7min, and redundant oxygen is removed. And (3) starting the substrate to rotate, regulating the evaporation current to 200A, enabling gold particles in the evaporation boat to be free of residues, turning off a heating power supply, and cooling the equipment along with a furnace for 30min to obtain the wafer-level imaging infrared enhanced absorption metal nano material with good adhesion effect, wherein the thickness of the gold-black film layer is 2 um.
The foregoing description of the preferred embodiments of the invention is merely illustrative of the invention and is not intended to be limiting. It should be noted that, for those skilled in the art, other equivalent modifications can be made in light of the technical teaching provided by the present invention, and the present invention can be implemented as the scope of protection.

Claims (6)

1. The preparation method of the infrared enhanced absorption metal nano material detector is characterized by comprising the following steps of:
(1) Sequentially preparing a Ti/Cr layer and an Au layer from top to bottom on the lower surface of the lithium tantalate wafer, and sequentially preparing the Ti/Cr layer and an Al layer from bottom to top on the upper surface of the lithium tantalate wafer;
(2) Preparing a high polymer adhesion layer on the surface of the Al layer; the polymer adhesive layer is 502 glue or AB glue, and the preparation method is fumigation or spin coating of the fumigation display cabinet;
(3) Placing a stainless steel mask plate above the lithium tantalate wafer;
(4) The gold black layer is prepared on the upper surface of the polymer adhesive layer by adopting high-purity gold particles as raw materials and adopting a thermal evaporation mode in an inert gas atmosphere.
2. The method according to claim 1, wherein the method of preparing in step (1) is a magnetron sputtering or thermal evaporation method.
3. The method according to claim 1, wherein the Ti/Cr layer thickness of step (1) is 1 to 20nm, the Au layer thickness is 100 to 500nm, and the Al layer thickness is 200 to 800nm.
4. The method of claim 1, wherein the step (4) is thermal evaporation in a nitrogen atmosphere: placing high-purity gold particle raw material into molybdenum boat or tungsten boat, adjusting distance between lithium tantalate wafer and molybdenum boat or tungsten boat to 1-10cm, extracting vacuum degree to below 1Pa, and keeping introducing N 2 Regulating N for 5-10min 2 The air pressure is 1500Pa-4000Pa, the current is adjusted to 10A-200A, and gold particles in the molybdenum boat or the tungsten boat are evaporated until no gold material remains, so that a gold black layer is obtained.
5. The method of claim 1, wherein the gold black layer has a thickness of 200nm to 5um.
6. An infrared enhanced absorption metal nanomaterial detector made by the method of manufacture of claim 1, wherein the material comprises: the lithium tantalate chip, the lower surface of lithium tantalate chip is equipped with Ti/Cr layer and Au layer in proper order from top to bottom, the upper surface of lithium tantalate chip is equipped with Ti/Cr layer and Al layer, polymer adhesion layer and gold black layer in proper order from bottom to top.
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