CN109971199A - A kind of resin base acoustic matching layer material and preparation method thereof - Google Patents

A kind of resin base acoustic matching layer material and preparation method thereof Download PDF

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Publication number
CN109971199A
CN109971199A CN201910227296.3A CN201910227296A CN109971199A CN 109971199 A CN109971199 A CN 109971199A CN 201910227296 A CN201910227296 A CN 201910227296A CN 109971199 A CN109971199 A CN 109971199A
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matching layer
acoustic matching
resin
resin base
layer material
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赵雷
陈辉
方伟
何漩
李薇馨
曾祥会
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0887Tungsten
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213Oxides; Hydroxides of metals of rare earth metal of cerium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Transducers For Ultrasonic Waves (AREA)
  • Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)

Abstract

The present invention relates to a kind of resin base acoustic matching layer materials and preparation method thereof.Its technical solution is: using the hollow sphere of the resin of 50~90wt% and 10~50wt% as raw material, the curing agent of the additional 20~30wt% of raw material and the additive of 1~5wt% mix 3~15min to get pug;By the pug cast molding, 3~10h is spontaneously dried, demoulding, toast 12 under the conditions of 60~120 DEG C~for 24 hours, resin base acoustic matching layer material is made.Present invention process is simply and can continuous production, obtained resin base acoustic matching layer material has the characteristics that processable thickness, light-weight, high temperature resistant, the conducting of corrosion-resistant, efficient and broadband, realizes in aerospace, High aititude geological mapping, deep-sea detecting, polar region scientific research and unpiloted development and demand.With extensive society and economic value.

Description

A kind of resin base acoustic matching layer material and preparation method thereof
Technical field
The invention belongs to acoustic matching layer field of material technology.More particularly to a kind of resin base acoustic matching layer material and its preparation Method.
Background technique
Ultrasonic transducer is that the electric signal of alternation is converted into acoustical signal in ultrasonic frequency range or turns acoustical signal It is changed to the energy conversion device of electric signal, ultrasonic transducer is one of basis and crucial acoustic element.Ultrasonic transducer is main Including shell, matching layer, that is, sound window, piezoceramic disc energy converter, backing, outgoing cable composition.Ultrasonic transducer usually works Near its resonance frequency, equivalent impedance can change with the working condition of ultrasonic transducer and the variation of environment.
With the progress of investigation of materials, ultrasonic transducer is being constantly progressive.French scientist Langevin designed in 1916 The sandwich transducer applied to underwater operation be the ultrasonic transducer occurred earliest in history, the pressure that this energy converter uses Electric material is quartz crystal, applies piezoelectric material on sonar for the first time.Magnetostriction materials are to prepare energy converter Another common used material, mainly include metal materials and the ferrite ceramic material such as nickel, ferrocobalt.It is prepared based on them Magnetostrictive transducer have the characteristics that structure is simple, impact resistance is strong, performance is stable, be particularly suitable for work in the presence of a harsh environment Make, is a kind of with high-intensitive high-power energy converter.But since its electromechanical conversion efficiency is low, the range being applied at present is got over Come smaller.Only good sounding (piezoelectricity) material, which is difficult to ensure, prepares high-performance ultrasound energy converter, because of piezoelectric material and spy The acoustic impedance mismatch surveyed between medium will be such that acoustic energy flow does not transmit effectively.By taking medical or underwater acoustic transducer as an example, when no When with layer coupling, 18% or so of the total sound energy of the acoustic energy Zhan being transferred in human body or water.
Acoustic matching material is mainly based on resin-based materials at present.Main preparation means are combined true with casting method and spin-coating method Based on empty technology, on direct pouring or spin coating basis material.The frequency given for one, the thickness of matching layer should for λ/ 4, and its acoustic impedance is the geometrical mean of piezoelectric material and destination organization acoustic impedance product.Casting method and spin-coating method cannot be accurate Control matching layer thickness.In addition, by casting and spin-coating method formed matching layer material, use scope is single, can not replace and Maintenance causes ultrasonic transducer use scope and time limit insufficient.With current preparation process, the design of matching layer is still with single layer Based on, at most develop to bilayer.To find out its cause, although the matching essentially consisted in more than two layers can further change to a certain extent The overall bandwidth and detection sensitivity of kind energy converter, but process aspect bring is difficult and limits to, and makes to deposit between multiple interfaces Imperfect bonding, gas hole defect, dust impurities the problems such as highlight, significantly counteract that multi-layer Matched bring is limited to be changed It is kind.Therefore, the single or double layer matching layer of correlative study unit production, intrinsic bandwidth only up to reach in the world at present 80% or so, seriously affect the use scope and sensitivity of ultrasonic transducer.
" a kind of ultrasonic transducer matching layer and its manufacturing method " (CN 107107108A) patented technology, discloses one kind The acoustic matching material that thickness is limited by the monodisperse particles single layer limited, the patented technology have the disadvantage in that (1) thickness by The monodisperse particles single layer of restriction limits, and causes thickness uncontrollable;(2) monodisperse particles are rigid particles, sound transitivity Can be excellent, and the interfacial bonding property of particle and resin is poor, causes ultrasonic transducer spirit lightness low.A kind of " wedgelike acoustic matching The production method of layer " (CN 103796149A) patented technology, discloses a kind of using the quartz micro needle with Wedge structure as mould Plate, by loading epoxy resin, wedgelike acoustic matching layer is made in the methods of erodent template, and method is sufficiently complex, and needs Using hydrofluoric acid solution, it is unfavorable for industrial production.
Summary of the invention
The present invention is directed to overcome prior art defect, and it is an object of the present invention to provide a kind of simple process and energy quantity-produced resin Base acoustic matching layer material preparation method, this method preparation resin base acoustic matching layer material filler and resin between associativity it is good, Thickness is processable, light-weight, intensity is big, high temperature resistant, the conducting of corrosion-resistant, cold-resistant, efficient and broadband.
To achieve the above object, the technical scheme adopted by the invention is that: with the resin of 50~90wt% and 10~ The hollow sphere of 50wt% be raw material, the curing agent of the additional 20~30wt% of raw material and the additive of 1~5wt%, mixing 3~ 15min is to get pug;By the pug cast molding, 3~10h is spontaneously dried, demoulding toasts 12 under the conditions of 60~120 DEG C ~for 24 hours, resin base acoustic matching layer material is made.
The resin is fluoro- Si modification nanometer water resin, silicon dioxide modified acrylic resin, aluminum oxide are modified One of epoxy resin, half silicone-modified bisphenol A type epoxy resin and silicon titanium hybridization epoxy resin.
The hollow sphere is in alumina hollow ball, hollow silica ball, magnesia hollow sphere and calcium oxide hollow sphere One kind.
The curing agent is in dimethyl carbonate, diethyl carbonate, methyl esters, ethyl ester, butyl ester, glycol ester and glyceride It is a kind of.
The additive is one of copper powder, tungsten powder, cerium oxide and yttrium oxide.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
The present invention is using resin and hollow sphere as raw material, additional curing agent and additive, mixing, and cast molding is dry, takes off Mould toasts to get resin base acoustic matching layer material.Therefore preparation process is simply and can continuous production.
The present invention uses cast molding method, and the later period can form prefabricated component by Precision Machining, and thickness can design tune Whole, resin base acoustic matching layer material can be adjusted at any time, replaces and be overhauled in practical application.Therefore, traditional casting method is solved With spin-coating method combination vacuum technique directly caused by preparing matching layer on piezoelectric ceramics complex process, overhaul in practical application Key technology difficulty that is difficult and can not replacing, therefore preparation process is simple and thickness is processable.
The present invention overcomes conventional filler (inorganic non-metallic material, plastics, tungsten powder) scope of applications single, performance-adjustable Difference, resin base acoustic matching material acoustic impedance range is narrow, precision is low and the key technology difficulties such as poor controllability.It is filled out using hollow sphere Material, sound wave easily enter hollow ball material, can be decayed by the aperture of hollow ball material depths and absorb, to improve resin base sound Acoustical behavior with layer material can reduce interface cohesion effect between filler and resin using organic-inorganic hybrid resin.With this Meanwhile organic-inorganic hybrid resin has the advantages that high temperature resistant, corrosion resistant so that resin base acoustic matching layer material it is resistant to high temperatures, Corrosion resistance is improved.Therefore resin base acoustic matching layer material is prepared in addition to light-weight, high temperature resistant, corrosion-resistant, resistance to tight The advantages that cold, efficient, broadband is connected realizes in the row such as aerospace, High aititude geological mapping, deep-sea detecting, polar region scientific research The development and demand of industry have extensive society and economic value.
Therefore, the present invention has the characteristics that simple process and energy continuous production, prepared resin base acoustic matching layer material Filler with associativity between resin is good, thickness is processable, light-weight, high temperature resistant, corrosion-resistant, efficient and broadband are connected, realize In aerospace, High aititude geological mapping, deep-sea detecting, polar region scientific research and unpiloted development and demand.With extensive Society and economic value.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limit of the scope of the present invention System.
Embodiment 1
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 50~60wt% and 40~50wt% as raw material, the additional 20~24wt%'s of raw material The additive of curing agent and 1~2wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 3~ 5h, demoulding, under the conditions of 60~80 DEG C toast 22~for 24 hours, be made resin base acoustic matching layer material.
The resin is fluoro- Si modification nanometer water resin.
The hollow sphere is alumina hollow ball.
The curing agent is dimethyl carbonate.
The additive is copper powder.
Embodiment 2
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 60~70wt% and 30~40wt% as raw material, the additional 22~26wt%'s of raw material The additive of curing agent and 2~3wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 5~ 18~22h is toasted in 7h, demoulding under the conditions of 80~100 DEG C, and resin base acoustic matching layer material is made.
The resin is fluoro- Si modification nanometer water resin.
The hollow sphere is hollow silica ball.
The curing agent is diethyl carbonate.
The additive is tungsten powder.
Embodiment 3
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 70~80wt% and 20~30wt% as raw material, the additional 24~28wt%'s of raw material The additive of curing agent and 3~4wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 7~ 16~18h is toasted in 10h, demoulding under the conditions of 100~120 DEG C, and resin base acoustic matching layer material is made.
The resin is silicon dioxide modified acrylic resin.
The hollow sphere is magnesia hollow sphere.
The curing agent is methyl esters.
The additive is cerium oxide.
Embodiment 4
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 80~90wt% and 10~20wt% as raw material, the additional 26~30wt%'s of raw material The additive of curing agent and 4~5wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 3~ 12~16h is toasted in 5h, demoulding under the conditions of 60~80 DEG C, and resin base acoustic matching layer material is made.
The resin is aluminum oxide modified epoxy.
The hollow sphere is calcium oxide hollow sphere.
The curing agent is ethyl ester.
The additive is yttrium oxide.
Embodiment 5
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 50~60wt% and 40~50wt% as raw material, the additional 21~24wt%'s of raw material The additive of curing agent and 1~2wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 5~ 16~18h is toasted in 7h, demoulding under the conditions of 80~100 DEG C, and resin base acoustic matching layer material is made.
The resin is half silicone-modified bisphenol A type epoxy resin.
The hollow sphere is alumina hollow ball.
The curing agent is butyl ester.
The additive is copper powder.
Embodiment 6
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 60~70wt% and 30~40wt% as raw material, the additional 24~27wt%'s of raw material The additive of curing agent and 1~2wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 7~ 18~22h is toasted in 10h, demoulding under the conditions of 100~120 DEG C, and resin base acoustic matching layer material is made.
The resin is silicon titanium hybridization epoxy resin.
The hollow sphere is hollow silica ball.
The curing agent is glycol ester.
The additive is tungsten powder.
Embodiment 7
A kind of resin base acoustic matching layer material and preparation method thereof.Preparation method described in the present embodiment is:
Using the hollow sphere of the resin of 70~80wt% and 20~30wt% as raw material, the additional 26~30wt%'s of raw material The additive of curing agent and 1~2wt% mixes 3~15min to get pug;By the pug cast molding, spontaneously dry 3~ 5h, demoulding, under the conditions of 100~120 DEG C toast 22~for 24 hours, be made resin base acoustic matching layer material.
The resin is silicon titanium hybridization epoxy resin.
The hollow sphere is alumina hollow ball.
The curing agent is glyceride.
The additive is cerium oxide.
Present embodiment has following good effect compared with prior art:
Present embodiment is using resin and hollow sphere as raw material, additional curing agent and additive, mixing, cast molding, Dry, demoulding is toasted to get resin base acoustic matching layer material.Therefore preparation process is simply and can continuous production.
Present embodiment uses cast molding method, and the later period can form prefabricated component by Precision Machining, and thickness can To design adjustment, resin base acoustic matching layer material can be adjusted at any time, replaces and be overhauled in practical application.Therefore, biography is solved System casting method and spin-coating method combination vacuum technique directly caused by preparing matching layer on piezoelectric ceramics complex process, actually answer Key technology difficulty that is difficult with middle maintenance and can not replacing, therefore preparation process is simple and thickness is processable.
Present embodiment overcome conventional filler (inorganic non-metallic material, plastics, tungsten powder) scope of application it is single, can Regulation performance is poor, resin base acoustic matching material acoustic impedance range is narrow, precision is low and the key technology difficulties such as poor controllability.Use sky Bulbus cordis filler, sound wave easily enter hollow ball material, can be decayed by the aperture of hollow ball material depths and absorb, to improve resin The acoustical behavior of base acoustic matching layer material can be reduced interface cohesion between filler and resin and be imitated using organic-inorganic hybrid resin It answers.At the same time, organic-inorganic hybrid resin has the advantages that high temperature resistant, corrosion resistant, so that resin base acoustic matching layer material Resistant to high temperatures, corrosion resistance is improved.Therefore resin base acoustic matching layer material is prepared in addition to light-weight, high temperature resistant, corrosion resistant The advantages that erosion, cold-resistant, efficient, broadband are connected, realizes in aerospace, High aititude geological mapping, deep-sea detecting, polar region section It the development and demand of industries such as grinds, there is extensive society and economic value.
Therefore, present embodiment has the characteristics that simple process and energy continuous production, prepared resin base sound Associativity is good between filler and resin with layer material, thickness is processable, light-weight, high temperature resistant, corrosion-resistant, efficient and broadband are led It is logical, it realizes in aerospace, High aititude geological mapping, deep-sea detecting, polar region scientific research and unpiloted development and demand.Tool There are extensive society and economic value.

Claims (5)

1. a kind of preparation method of resin base acoustic matching layer material, which is characterized in that with the resin of 50~90wt% and 10~ The hollow sphere of 50wt% be raw material, the curing agent of the additional 20~30wt% of raw material and the additive of 1~5wt%, mixing 3~ 15min is to get pug;By the pug cast molding, 3~10h is spontaneously dried, demoulding toasts 12 under the conditions of 60~120 DEG C ~for 24 hours, resin base acoustic matching layer material is made;
The resin is fluoro- Si modification nanometer water resin, silicon dioxide modified acrylic resin, aluminum oxide modified epoxy One of resin, half silicone-modified bisphenol A type epoxy resin and silicon titanium hybridization epoxy resin.
2. the preparation method of resin base acoustic matching layer material according to claim 1, it is characterised in that the hollow sphere is One of alumina hollow ball, hollow silica ball, magnesia hollow sphere and calcium oxide hollow sphere.
3. the preparation method of resin base acoustic matching layer material according to claim 1, it is characterised in that the curing agent is One of dimethyl carbonate, diethyl carbonate, methyl esters, ethyl ester, butyl ester, glycol ester and glyceride.
4. the preparation method of resin base acoustic matching layer material according to claim 1, it is characterised in that the additive is One of copper powder, tungsten powder, cerium oxide and yttrium oxide.
5. a kind of resin base acoustic matching layer material, it is characterised in that the resin base acoustic matching layer material is according to claim 1 Resin base acoustic matching layer material prepared by the preparation method of resin base acoustic matching layer material described in any one of~4.
CN201910227296.3A 2019-03-25 2019-03-25 A kind of resin base acoustic matching layer material and preparation method thereof Withdrawn CN109971199A (en)

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EP4137526A1 (en) * 2021-08-17 2023-02-22 ThreeBond Co., Ltd. Thermally conductive resin composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4137526A1 (en) * 2021-08-17 2023-02-22 ThreeBond Co., Ltd. Thermally conductive resin composition

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Application publication date: 20190705