CN107189286B - A kind of oxidation resistant hybrid particulates and its polymer matrix composite - Google Patents
A kind of oxidation resistant hybrid particulates and its polymer matrix composite Download PDFInfo
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- CN107189286B CN107189286B CN201610143633.7A CN201610143633A CN107189286B CN 107189286 B CN107189286 B CN 107189286B CN 201610143633 A CN201610143633 A CN 201610143633A CN 107189286 B CN107189286 B CN 107189286B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2201/003—Additives being defined by their diameter
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The present invention provides a kind of oxidation resistant hybrid particulates and its polymer matrix composites.By the total weight of the oxidation resistant hybrid particulates be 100 parts by weight in terms of, which includes the anti oxidation layer of -0.5 parts by weight of the ferroelectric ceramic grain of -90 parts by weight of 20 parts by weight, the base metal particle of -80 parts by weight of 10 parts by weight and 0.15 parts by weight；The size of metallic particles is less than the size of ferroelectric ceramic grain；Base metal particle is deposited on ferroelectric ceramic grain surface, forms ferroelectric ceramics-metal hybrid particle, and anti oxidation layer is coated on the ferroelectric ceramics-metal hybrid particle surface, forms oxidation resistant hybrid particulates.Polymer matrix composite provided by the invention includes the polymer of 20wt%-80wt% and the above-mentioned oxidation resistant hybrid particulates of 20wt%-80wt%.Oxidation resistant hybrid particulates of the invention and polymer matrix composite have high dielectric constant, low loss factors, good inoxidizability and mechanical performance.
Description
Technical field
The present invention relates to a kind of hybrid particulates and its polymer matrix composite more particularly to a kind of oxidation resistant hydridization
Grain and its polymer matrix composite, belong to hybrid particulates technical field.
Background technique
New material with high dielectric constant and low-dielectric loss occupies critically important ground in entire electronic industry field
Position, the high dielectric material especially used at higher frequencies have become a kind of reduction device volume, are further miniaturized
Key means.
Now, in traditional electronic system, Passive components, passive electronic quantity be gradually more than active collection
At circuit, quantity has been as many as several times of the latter, and occupation rate has been over 70% on fixed circuit substrate.Passive member device
Part has become major obstacle of the electronic system in miniaturization fall process.In order to improve passive device efficiency, passive device is reduced
Quantity, reduces board area, and the development of passive device technology will gradually become embedment by traditional type stand alone type passive device
The functionalized design of formula passive device.In chip package, the integrated technology of passive device has following advantage, preferably electricity
Performance, higher reliability, lower cost and more alternative design schemes.
At present be suitable in the high dielectric of buried capacitor device, the material of low loss dielectric mainly include ferroelectric ceramics/
Polymer composites, conductive filler/polymer material, fully organic high-dielectric composite material, conductive particle@insulating layer/polymerization
Object composite material and ceramics-conductive particle/polymer composites, above-mentioned all kinds of dielectric materials respectively have advantage and disadvantage, but cannot
Fully meet demand of the buried capacitor to dielectric material.
Wherein, a large amount of ferroelectric ceramic grain is introduced into polymer by ferroelectric ceramics/polymer composites, including titanium
Sour barium (BaTiO3), CaCu 3 Ti 4 O (CCTO), barium strontium titanate (BaSrTiO3) etc. with very high dielectric constant ferroelectric ceramics,
But in order to meet corresponding mechanical performance, it is necessary to polymeric substrates are introduced, this results in the sharply decline of dielectric constant, in order to
Dielectric constant is improved, this kind of material can only be the content for further increasing ceramics, can so reduce the mechanicalness of composite material again
Energy；Conductive filler/polymer material by various conductive particles or fiber such as carbon nanotube (CNT), stainless steel fibre (SSF), silver,
Aluminium etc. is introduced into polymer matrix to improve dielectric constant, since there are seep effects, when packing volume mark reaches centainly
When value, conductive filler is in contact with each other, and forms conductive path, therefore conductivity and dielectric loss also steeply rise, and causes to meet not
Low-loss requirement；Full stress-strain dielectric composite material has excellent mechanical performance, but the conductive polymer material introduced is such as
The easy reunions such as polyaniline (PANI), disperse in the base uneven and cause unevenly to be lost, buried capacitor material can not be met
The requirement of material；Conductive particle@insulating layer/polymer material is a kind of dielectric substance for studying more perfect, this insulation
The nucleocapsid structure of layer coated with conductive particle can not only prevent the formation of conductive path, and polarizability is higher, to a certain extent
The dielectric constant of raising again can inhibit loss in reduced levels, but as buried capacitor is (on bus plane first surface and stratum the
Add dielectric material between one surface, printed circuit board be pressed together) development, the requirement to energy storage density is further
It improves, so that requiring the dielectric constant of material higher and higher；Ceramics-conductive particle/polymer composites are by conductive
Grain, in the high hybrid particulates of ceramic grain surface, is then introduced in polymer matrix by certain method dispersed deposition, this
Class material use ferroelectric ceramics has the property of high dielectric, and control conductive particle obtains having height in its surface distribution situation
The dielectric material of dielectric constant, low loss factors, but the metallic particles for being dispersed in ferroelectric ceramics surface exists and is easily oxidized
Problem (especially when metallic particles be price it is lower, suitable for large-scale application base metal when), so as to cause polarizability decline,
Dielectric constant declines therewith, to limit the use of this kind of material.
Based on this, it is necessary to provide a kind of with high dielectric constant, low loss factors, good antioxygenic property and machinery
The composite material of performance.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of oxidation resistant ferroelectric ceramics-metal is miscellaneous
Change the composite material of particle and its polymer matrix.Contain above-mentioned ferroelectric ceramics-metal hybrid particle polymer matrix composite
With good dielectric properties and antioxygenic property.
In order to achieve the above technical purposes, the present invention is by coating one layer of antioxygen on ceramics-base metal hybrid particulates surface
The means for changing layer, solve the problems, such as that base metal is easily oxidized in forming process, impart composite material with good Jie
Electrical property and antioxygenic property.The present invention provides a kind of oxidation resistant hybrid particulates, with the total of the oxidation resistant hybrid particulates
Weight is 100 parts by weight meters, which includes the ferroelectric ceramic grain of -90 parts by weight of 20 parts by weight, 10 weights
Measure the anti oxidation layer of -0.5 parts by weight of base metal particle and 0.15 parts by weight of -80 parts by weight of part；
Wherein, the size of base metal particle is less than the size of ferroelectric ceramic grain；
Base metal particle is deposited on ferroelectric ceramic grain surface, forms ferroelectric ceramics-metal hybrid particle, anti oxidation layer packet
Ferroelectric ceramics-metal hybrid particle surface is overlayed on, oxidation resistant hybrid particulates are formed.
In oxidation resistant hybrid particulates provided by the invention, it is preferable that the partial size of the base metal particle used is 15nm-
35nm, the partial size of the ferroelectric ceramic grain used is 50nm-500nm.
In oxidation resistant hybrid particulates provided by the invention, it is preferable that base metal particle is grown by heterogeneous nucleation
It is deposited on ferroelectric ceramic grain surface.
In oxidation resistant hybrid particulates provided by the invention, according to difference is required, base metal particle is with different depositions
Rate is deposited on ferroelectric ceramic grain surface, it is preferable that deposition of the base metal particle on ferroelectric ceramic grain surface is 5%-
85%.
In oxidation resistant hybrid particulates provided by the invention, it is preferable that the base metal particle of use includes aluminium nanometer
One of grain, iron nano-particle, zinc nanoparticles, copper nano particles, nano nickel particles, tin nanoparticles and tungsten nano particle
Or several combination.
In oxidation resistant hybrid particulates provided by the invention, it is preferable that the ferroelectric ceramic grain of use includes copper titanate
In calcium ceramic particle, barium titanate ceramics particle, lead titanate ceramics particle, barium-strontium titanate ceramic particle and lead zirconate-titanate ceramic particle
One or more of combinations.
In oxidation resistant hybrid particulates provided by the invention, it is preferable that the raw material of the anti oxidation layer of use, which forms, includes
The combination of one or more of polyvinylpyrrolidone, polyethylene glycol, oleyl amine and higher fatty acids；
In oxidation resistant hybrid particulates provided by the invention, it is preferable that the higher fatty acids of use includes palmitinic acid, hard
The combination of one or more of ester acid, oleic acid, linolenic acid and arachidic acid.
In oxidation resistant hybrid particulates provided by the invention, the base metal particle of use can be circular granular, can also
To be the particle of irregular shape.
The present invention provides the preparation method of above-mentioned oxidation resistant hybrid particulates, the preparation method the following steps are included:
The salting liquid of base metal is dissolved in reducing agent, the raw material composition and ferroelectric ceramic grain of the anti oxidation layer is added；
10min-60min is stirred with the speed of 200r/min-1600r/min at room temperature, ultrasonic 10min-120min is obtained
Suspension；
By the suspension, oil bath 10min-240min, oil bath process are passed through protective gas at 120 DEG C -250 DEG C, reaction
Continue to stir 10min-60min after the completion and is continually fed into protective gas；
After cleaned, centrifugation, separation, cleaning treatment, 1h-12h is dried under vacuum conditions, is obtained described oxidation resistant miscellaneous
Change particle.
Specific embodiment according to the present invention, using protective gas commonly used in the art, generally nitrogen, argon
Gas.
In the preparation method of oxidation resistant hybrid particulates provided by the invention, it is preferable that the raw material of anti oxidation layer forms
Additive amount be ferroelectric ceramic grain and base metal particle gross mass 0.15%-0.5%.
In the preparation method of oxidation resistant hybrid particulates provided by the invention, it is preferable that the salt of the base metal of use is molten
Liquid includes at least one of the organic slat solution of base metal, the inorganic salt solution of base metal and onium hydroxide solution of base metal.
In the preparation method of oxidation resistant hybrid particulates provided by the invention, it is preferable that the reducing agent of use includes Portugal
At least one of grape sugar, polyalcohol and ascorbic acid.
The present invention also provides a kind of polymer matrix composites, are with the gross mass of the polymer matrix composite
100wt% meter, the polymer matrix composite include 20wt%-80wt% polymer and 20wt%-80wt% it is anti-oxidant
Hybrid particulates；
Wherein, the oxidation resistant hybrid particulates used is above-mentioned oxidation resistant hybrid particulates.
In polymer matrix composite provided by the invention, it is preferable that the polymer of use include polyvinylidene fluoride,
At least one of epoxy resin, polyimides, phenolic resin, polyester resin, rubber and double Malaya's amide resins.
In polymer matrix composite provided by the invention, it is preferable that the polymer matrix composite is in frequency
1kHz, dielectric constant at room temperature are 20-250.
In polymer matrix composite provided by the invention, it is preferable that the polymer matrix composite is in frequency
1kHz, dielectric constant at room temperature are 50-250.
The present invention provides the preparation method of above-mentioned polymer matrix composite, the preparation method the following steps are included:
It disperses above-mentioned oxidation resistant hybrid particulates in the solution dissolved with the polymer, ultrasonic agitation to dividing completely
It dissipates, directly heats solidification by product requirement, perhaps film after hot-forming after being dried in vacuo or ball milling, obtains institute
State polymer matrix composite.
In oxidation resistant hybrid particulates of the invention, base metal particle is similar to the lattice types of ferroelectric ceramic grain,
Lattice constant is close, and base metal particle, on ferroelectric ceramic grain surface, makes oxidation resistant hydridization by heterogeneous nucleation acting growth
The stable structure of particle, application reliability are high.
In polymer matrix composite provided by the invention, discrete point in the polymer of antioxidative hybrid particulates
Cloth, polymer link together what antioxidative hybrid particulates dispersed, prevent antioxidative hybrid particulates from reuniting, antioxygen
The surface oxidation-resistant layer of the hybrid particulates for the property changed has blocked the formation of conductive path, has both improved Jie of polymer matrix composite
Electric constant, and the increase of fissipation factor is effectively inhibited, and make polymer matrix composite that there is good mechanicalness
Energy.
Oxidation resistant hybrid particulates of the invention and its polymer matrix composite have the following beneficial effects:
Oxidation resistant hybrid particulates of the invention have high dielectric constant, low loss factors and good inoxidizability；
The preparation process of the preparation method of oxidation resistant hybrid particulates of the invention is simple, by chemical method in base metal
Surface has coated one layer of anti oxidation layer, can play the role of starvation, prevents base metal from reacting with oxygen, solves low-priced gold
The problem of category is easily oxidized in forming process；
Polymer matrix composite high dielectric constant, low loss factors, good inoxidizability and machine provided by the invention
Tool performance；
The process flow of the preparation method of polymer matrix composite provided by the invention is simple, and condition is easily-controllable, qualification rate
Height, at low cost, with short production cycle, shaping efficiency is high, is suitable for mechanical automation and produces.
Detailed description of the invention
Fig. 1 is the preparation flow figure of the antioxidative hybrid particulates of embodiment 1.
Fig. 2 is the structural schematic diagram in polymer matrix composite with antioxidative hybrid particulates.
Fig. 3 is scanning electron microscope (SEM) figure of the antioxidative hybrid particulates of embodiment 1.
Fig. 4 is transmission electron microscope (TEM) figure of the antioxidative hybrid particulates of embodiment 1.
Fig. 5 a is X-ray energy spectrum antioxidant assay (XPS) figure of the antioxidative hybrid particulates of embodiment 1.
Fig. 5 b is that the antioxidative hybrid particulates of embodiment 1 place 30 days X-ray energy spectrum antioxidant assays (XPS)
Figure.
Fig. 5 c is that the antioxidative hybrid particulates of embodiment 1 place 60 days X-ray energy spectrum antioxidant assays (XPS)
Figure.
Fig. 6 is the preparation flow figure of the polymer matrix composite of embodiment 3.
Fig. 7 is scanning electron microscope (SEM) figure of the polymer matrix composite of embodiment 3.
Fig. 8 a is the dielectric constant of slave 100Hz to the 1GHz of the polymer matrix composite of embodiment 3.
Fig. 8 b is the dielectric constant of slave 100Hz to the 1GHz of the polymer matrix composite of embodiment 3.
Fig. 8 c is the dielectric loss figure of slave 100Hz to the 1GHz of the polymer matrix composite of embodiment 3.
Fig. 8 d is the dielectric loss figure of slave 100Hz to the 1GHz of the polymer matrix composite of embodiment 3.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
Present embodiments providing one kind has antioxidative barium titanate-copper hybrid particulates, through the following steps that
It is prepared, specific preparation flow is as shown in Figure 1:
Macrogol 4000 (PEG-4000) 0.25g and CuSO4·5H2O 3.0g is dissolved in 100mL ethylene glycol, and ultrasound is stirred
20min is mixed, the BaTiO of 5.0g is added3(100nm), ultrasonic agitation 30min to solution become blue suspension；
Blue suspension is moved in three-necked flask and oil bath, oil bath temperature are 160-180 DEG C, reaction 2 as a child stopped
It heats and continues to stir 5min, whole process is continually fed into protective gas nitrogen；
Repeated washing-centrifugation-cleaning step 3-5 times after brown suspension is cooled to room temperature is dried in vacuo 12 at 30 DEG C
Hour, antioxidative hybrid particulates are obtained, structural schematic diagram is as shown in Figure 2.
By Fig. 3 SEM of the antioxidative hybrid particulates of the present embodiment (scheme) and Fig. 4 (the present embodiment it is antioxidative
The TEM of hybrid particulates schemes) as can be seen that the partial size for the base metal particle that the present embodiment uses is coated on hydridization for 15nm-35nm
The anti oxidation layer of particle surface with a thickness of 2nm-5nm.
The anti-oxidation characteristics for the antioxidative hybrid particulates that the present embodiment is prepared are as shown in Fig. 5 a, 5b, 5c, figure
5a, 5b, 5c are the antioxidative hybrid particulates copper 2P of the present embodiment2/3The XPS antioxidant assay figure of track, Fig. 5 a, 5b, 5c
Copper 2P after respectively preparing placement 0,30,60 day2/3Track XPS map.The sum that it can be seen from Fig. 5 a, 5b prepared by the same day is put
The XPS map set 30 days only has the characteristic peak of a 0 valence copper in 932.3eV, and without other satellites or miscellaneous peak, this is said
The copper of bright preparation is not oxidized to other valence states, and copper 2P after placing 60 days2/3There is divalent in 934.0eV in the XPS of track
The characteristic peak of copper, the prepared copper of this explanation have been oxidized to divalent.Thus may determine that the present embodiment be prepared it is anti-
The inoxidizability of the hybrid particulates of oxidation is 30-60 days.
Embodiment 2
Present embodiments providing one kind has antioxidative barium titanate-nickel hybrid particulates, through the following steps that system
For what is obtained:
Macrogol 4000 (PEG-4000) 0.25g and Ni (NO3)2·6H2O 3.5g is dissolved in 100mL ethylene glycol, ultrasound
30min is stirred, the BaTiO of 5.0g is added3(100nm), ultrasonic agitation 30min to solution become blue-green suspension；
Blue suspension is moved in three-necked flask and oil bath, oil bath temperature are 160-180 DEG C, reaction 2 as a child stopped
It heats and continues to stir 5min, whole process is continually fed into protective gas nitrogen；
Repeated washing-centrifugation-cleaning step 3-5 times after dark-brown suspension is cooled to room temperature, vacuum is dry at 30 DEG C
Dry 12 hours, obtain antioxidative hybrid particulates.
Embodiment 3
A kind of barium titanate-copper hybrid particulates/polyvinylidene fluoride composite material is present embodiments provided, is by following
What step was prepared, specific preparation flow is as shown in Figure 6:
Antioxidative barium titanate-copper hybrid particulates 0.2g, 0.4g, 0.6g, 0.7g, 0.8g in embodiment 1 is weighed, point
Jia Ru not be into the ethanol solution containing 0.8g, 0.6g, 0.4g, 0.3g, 0.2g Kynoar (PVDF), ultrasonic agitation
20min is placed in vacuum drying to being uniformly dispersed, by the mixing suspension of the oxidation resistant hybrid particulates containing different quality containing
12 hours in case；
It will be transferred to after the mixture grinding uniformly of different content after abundant drying into hot press die, it is hot at 170 DEG C
It is formed after pressure 15min, obtains the polymer matrix composite with different filer contents and good mechanical properties.
Fig. 7 be the barium titanate copper hybrid particulates mass fraction that the present embodiment is prepared be 60% barium titanate-copper/it is poly- inclined
The SEM of fluoride composite material schemes.
Fig. 8 a, 8b, 8c, 8d are different barium titanates-copper hybrid particulates content composite material that the present embodiment is prepared
Dielectric properties curve, wherein Fig. 8 a, 8b, be prepared for the present embodiment polymer matrix composite slave 100Hz to
The dielectric constant of 1GHz, Fig. 8 c, 8d are Jie of slave 100Hz to the 1GHz for the polymer matrix composite that the present embodiment is prepared
Electrical loss figure.It is found that the polymer matrix composite that is prepared of the present embodiment dielectric constant in 1kHz reaches as high as 150,
Corresponding dielectric loss factor is 0.15.
Embodiment 4
A kind of barium titanate-nickel hybrid particulates/polyvinylidene fluoride composite material is present embodiments provided, is by following
What step was prepared:
Weigh antioxidative barium titanate-nickel hybrid particulates 0.2g, 0.4g, 0.6g, 0.7g that embodiment 2 is prepared,
0.8g is added separately in the ethanol solution containing 0.8g, 0.6g, 0.4g, 0.3g, 0.2g Kynoar (PVDF), ultrasound
The mixing suspension of anti-oxidant hybrid particulates containing different quality containing is placed in vacuum to after being uniformly dispersed and done by stirring 20min
12 hours in dry case；
It will be transferred to after the mixture grinding uniformly of different content after abundant drying into hot press die, it is hot at 170 DEG C
It is formed after pressure 15min, obtains the polymer matrix composite with different filer contents and good mechanical properties.
Above embodiments explanation, oxidation resistant hybrid particulates of the invention and polymer matrix composite have high dielectric normal
Number, low loss factors, good inoxidizability and mechanical performance.
Claims (10)
1. a kind of preparation method of oxidation resistant hybrid particulates, which is characterized in that the preparation method the following steps are included:
By at least one of the organic slat solution of base metal, the inorganic salt solution of base metal and hydroxide solution of base metal
It is dissolved in reducing agent, the raw material composition and ferroelectric ceramic grain of anti oxidation layer is added；
10min-60min is stirred with the speed of 200r/min-1600r/min at room temperature, ultrasonic 10min-120min is obtained suspended
Liquid；
By the suspension, oil bath 10min-240min, oil bath process are passed through protective gas at 120 DEG C -250 DEG C, and reaction is completed
After continue to stir and 10min-60min and be continually fed into protective gas；
After cleaned, centrifugation, separation, cleaning treatment, 1h-12h is dried under vacuum conditions, obtains the oxidation resistant hydridization
Grain；
The base metal particle is deposited on the ferroelectric ceramic grain surface, forms ferroelectric ceramics-metal hybrid particle, described anti-
Oxide layer is coated on the ferroelectric ceramics-metal hybrid particle surface, forms the oxidation resistant hybrid particulates；
The partial size of the base metal particle is 15nm-35nm, and the partial size of the ferroelectric ceramic grain is 50nm-500nm；
The additive amount of the raw material composition of the anti oxidation layer is the ferroelectric ceramic grain and base metal particle gross mass
0.15%-0.5%；
The raw material composition of the anti oxidation layer includes one in polyvinylpyrrolidone, polyethylene glycol, oleyl amine and higher fatty acids
Kind or several combinations.
2. the preparation method of oxidation resistant hybrid particulates according to claim 1, which is characterized in that base metal particle is aluminium
In nano particle, iron nano-particle, zinc nanoparticles, copper nano particles, nano nickel particles, tin nanoparticles and tungsten nano particle
One or more of combinations.
3. the preparation method of oxidation resistant hybrid particulates according to claim 1, which is characterized in that the reducing agent is Portugal
At least one of grape sugar, polyalcohol and ascorbic acid.
4. the preparation method of oxidation resistant hybrid particulates according to claim 1, which is characterized in that the base metal particle
Deposition on the ferroelectric ceramic grain surface is 5%-85%.
5. the preparation method of oxidation resistant hybrid particulates according to claim 1, which is characterized in that the ferroelectric ceramics
Grain is calcium copper titanate ceramics particle, barium titanate ceramics particle, lead titanate ceramics particle, barium-strontium titanate ceramic particle and lead zirconate titanate
The combination of one or more of ceramic particle.
6. the preparation method of oxidation resistant hybrid particulates according to claim 1, which is characterized in that the higher fatty acids
For the combination of one or more of palmitinic acid, stearic acid, oleic acid, linolenic acid and arachidic acid.
7. a kind of polymer matrix composite, which is characterized in that the gross mass with the polymer matrix composite is 100wt%
Meter, which includes the polymer of 20wt%-80wt% and the oxidation resistant hydridization of 20wt%-80wt%
Grain；
Wherein, the oxidation resistant hybrid particulates are the preparation of oxidation resistant hybrid particulates described in any one of claims 1-6
What method was prepared.
8. polymer matrix composite according to claim 7, which is characterized in that the polymer includes gathering inclined difluoro second
At least one of alkene, epoxy resin, polyimides, phenolic resin, polyester resin, rubber and double Malaya's amide resins.
9. polymer matrix composite according to claim 7 or 8, which is characterized in that the polymer matrix composite exists
Frequency is 1kHz, dielectric constant at room temperature is 20-250.
10. polymer matrix composite according to claim 9, which is characterized in that the polymer matrix composite is in frequency
Rate is 1kHz, dielectric constant at room temperature is 50-250.
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| CN108212136B (en) * | 2018-01-30 | 2020-08-04 | 河北工业大学 | Preparation method of flower-shaped directional SrTiO3 |
| CN108546124B (en) * | 2018-05-03 | 2021-07-30 | 景德镇市鑫惠康电子有限责任公司 | Preparation method of BCZT-based lead-free piezoelectric ceramic |
| CN110310829A (en) * | 2019-05-23 | 2019-10-08 | 深圳先进技术研究院 | Buried capacitor material, preparation method and printed wiring board |
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