CN114712250A - Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof - Google Patents

Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof Download PDF

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CN114712250A
CN114712250A CN202210247626.7A CN202210247626A CN114712250A CN 114712250 A CN114712250 A CN 114712250A CN 202210247626 A CN202210247626 A CN 202210247626A CN 114712250 A CN114712250 A CN 114712250A
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crown
ceramic
aluminum silicate
sodium aluminum
zinc oxide
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宁成云
肖才榕
谭帼馨
付如民
张哲琨
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South China University of Technology SCUT
Guangdong University of Technology
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South China University of Technology SCUT
Guangdong University of Technology
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/19Alkali metal aluminosilicates, e.g. spodumene
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/20Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/70Preparations for dentistry comprising inorganic additives
    • A61K6/71Fillers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention belongs to the technical field of crown and bridge repairing materials, and discloses crown and bridge repairing ceramic with efficient anti-deformation streptococcus, and preparation and application thereof. The method comprises the following steps: (1) carrying out ball milling on sodium aluminum silicate and nano zinc oxide to obtain sodium aluminum silicate powder doped with nano zinc oxide; by mass percentage, 97 to 99.5 percent of sodium aluminum silicate and 0.5 to 3 percent of nano zinc oxide; (2) and mixing the sodium aluminum silicate powder doped with the nano zinc oxide with a binder uniformly, aging, granulating, molding and calcining to obtain the efficient anti-streptococcus-mutans crown bridge repair ceramic. The crown bridge repairing ceramic with high-efficiency anti-streptococcus mutans has high-efficiency antibacterial efficiency on streptococcus mutans, and the added zinc oxide has no obvious hardness change on the sodium aluminum silicate ceramic substrate. The preparation method disclosed by the invention is simple in process, good in process controllability and high in repeatability, can be used for the crown and bridge repairing material, and has a relatively high popularization value.

Description

Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof
Technical Field
The invention belongs to the technical field of crown and bridge repairing materials, and particularly relates to a crown and bridge repairing ceramic with efficient anti-deformation streptococcus, and preparation and application thereof.
Background
Oral diseases, particularly dental caries and periodontal diseases are common frequently-occurring diseases and seriously affect the health of people. The crown bridge repairing material has made great progress with the continuous development, and the ceramic-based crown bridge repairing material and the forming technology have become a hot spot in recent ten years, wherein the sodium aluminum silicate ceramic is widely applied to the field of crown bridge repairing at present due to the matching of the mechanical property and the aesthetic property with natural teeth of a human body. However, the currently reported sodium aluminum silicate ceramics do not have antibacterial performance, and are easy to cause implantation failure due to bacterial infection in the early stage of implantation, so that the pain of a patient is further deepened, the time and the energy of the patient are wasted, and the treatment cost of the patient is increased. Streptococcus mutans is the largest proportion of the natural oral flora and has anaerobic properties, so that it is often aggregated to cause oral diseases such as dental caries. Therefore, the development of the sodium aluminosilicate ceramic with efficient anti-deformation streptococcus will greatly advance the field of crown bridge repair.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a preparation method of high-efficiency anti-streptococcus-deformation sodium aluminum silicate/nano zinc oxide composite ceramic (namely, crown bridge repair ceramic with high-efficiency anti-streptococcus-deformation).
The invention also aims to provide the high-efficiency anti-streptococcus-mutans sodium aluminum silicate/nano zinc oxide composite ceramic (namely the crown bridge repair ceramic with high-efficiency anti-streptococcus-mutans) obtained by the preparation method. The material of the invention has obvious antibacterial effect.
The invention further aims to provide application of the high-efficiency anti-streptococcus aluminum sodium silicate/nano zinc oxide composite ceramic (namely the crown and bridge repair ceramic with the high-efficiency anti-streptococcus) in the field of crown and bridge repair.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a crown bridge repairing ceramic with efficient anti-deformation streptococcus comprises the following steps:
(1) carrying out ball milling on sodium aluminum silicate and nano zinc oxide to obtain sodium aluminum silicate powder doped with nano zinc oxide; by mass percentage, 97 to 99.5 percent of sodium aluminum silicate and 0.5 to 3 percent of nano zinc oxide;
(2) mixing the sodium aluminum silicate powder doped with the nano zinc oxide with a binder uniformly, aging, granulating and molding to obtain molded sodium aluminum silicate/nano copper oxide;
(3) and calcining the formed sodium aluminum silicate/nano copper oxide to obtain the streptococcus mutans-resistant sodium aluminum silicate/nano copper oxide composite ceramic, namely the efficient streptococcus mutans-resistant crown and bridge repair ceramic.
In the step (1), absolute ethyl alcohol is added into sodium aluminum silicate and nano zinc oxide during ball milling; the ball milling time is 8-12h, and the ball milling speed is 300-450 rpm.
After ball milling, drying, grinding and sieving treatment are carried out.
The drying temperature is 40-75 ℃; the mesh number of the sieve is 60-100 meshes.
The dosage of the binder in the step (2) is 4-10% of the mass of the sodium aluminum silicate powder doped with the nano zinc oxide.
The binder consists of polyvinyl alcohol, glycerol and water; polyvinyl alcohol: glycerol: the mass ratio of water is (3-5): (1.5-2): 1.5: 30.
the aging time in the step (2) is 20-30 h.
The molding is to adopt a hand-pulling type press to perform primary pressing to form a blank body for molding, and then perform secondary pressing through cold isostatic pressing, wherein the pressure is 200-220 MPa; the molding time is 25-35 min.
The calcining conditions in the step (3) are as follows: the calcination temperature is 700 ℃ and 900 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 2-4 h.
The efficient anti-deformation streptococcus aluminum sodium silicate/nano zinc oxide composite ceramic is prepared by the method.
The high-efficiency anti-deformation streptococcus aluminum sodium silicate/nano zinc oxide composite ceramic is used for a medical crown and bridge repairing material, in particular to a crown and bridge repairing material.
The invention utilizes the sodium aluminum silicate ceramic material as a good dental crown repair material. By introducing zinc oxide nano particles, under the condition of not generating excessive influence on the self physical and chemical properties of the sodium aluminum silicate ceramic, the nano zinc oxide is contacted with bacteria to destroy the bacterial membrane, so that intracellular substances of the bacteria flow out to kill the bacteria and destroy genetic factors by utilizing the ion release of the zinc oxide; in addition, the nano zinc oxide can kill bacteria by generating active oxygen. Therefore, the material can quickly and efficiently kill the specific streptococcus mutans in the oral cavity, thereby avoiding the repair failure caused by bacterial infection in the early repair stage of the crown bridge repair material.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the preparation method of the invention has simple and convenient process; the process controllability is good, the repeatability is high, and the resources are saved; the ceramic provided by the invention can be used for quickly and efficiently killing streptococcus mutans, so that the repair failure caused by bacterial infection at the early stage of repair of the crown bridge repair material is avoided.
Drawings
FIG. 1 is a graph showing the antibacterial effect of sodium aluminum silicate (NAS) ceramics prepared in a comparative example on Streptococcus mutans;
FIG. 2 is a graph showing the antibacterial effect of 1 wt% ZnO-doped sodium aluminum silicate (NAS/1.0Zn) ceramic prepared in example 2 on Streptococcus mutans;
FIG. 3 is a graph showing the antibacterial effect of 3 wt% ZnO-doped sodium aluminum silicate (NAS/3.0Zn) ceramic prepared in example 4 on Streptococcus mutans;
FIG. 4 is a statistical chart of the count of the antibacterial plates of the ceramics prepared in comparative example, example 2 and example 4.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
Comparative example
Performing ball milling on the sodium aluminum silicate powder for 8 hours (adding absolute ethyl alcohol when the ball milling is performed, wherein the mass ratio of the powder to the absolute ethyl alcohol is 1:1.3), rotating at the speed of 300rpm, drying the slurry at 40 ℃, and then adding a binder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water: 3:1.5:1.5:30) accounting for 4% of the mass of the powder; grinding and sieving again (100 mesh), aging at 25 deg.C for 24 hr, tabletting, and isostatic pressing at 200MPa for 30 min; and (3) calcining the obtained sodium aluminum silicate/nano zinc oxide sheet at high temperature to obtain the ceramic, wherein the calcining temperature is 700 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2 h. FIG. 1 is a graph showing the antibacterial effect of sodium aluminum silicate (NAS) ceramic on Streptococcus mutans.
Compared with the blank group, the number of bacteria in the sodium aluminum silicate ceramic obtained by the comparative example is not obviously reduced, which shows that the sodium aluminum silicate ceramic does not have good antibacterial performance.
Example 1
Ball-milling 99.5% of sodium aluminum silicate and 0.5% of nano zinc oxide for 9 hours (adding absolute ethyl alcohol during ball-milling, wherein the mass ratio of the composite powder to the absolute ethyl alcohol is 1:1.3), rotating at 350rpm, drying the slurry at 40 ℃, and adding a binder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water) with the mass ratio of 5% of the composite powder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water: 4:2:1.5: 30); grinding and sieving (100 mesh), aging at 25 deg.C for 24 hr, tabletting, and isostatic pressing at 200MPa for 30 min; and (3) calcining the obtained sodium aluminum silicate/nano zinc oxide sheet at high temperature to obtain the ceramic, wherein the calcining temperature is 750 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2.5 h.
Example 2
Ball-milling sodium aluminum silicate and nano zinc oxide according to the mass ratio of 99% to 1% for 10h (adding absolute ethyl alcohol during ball milling, wherein the mass ratio of the composite powder to the absolute ethyl alcohol is 1:1.3), rotating at 400rpm, drying the slurry at 40 ℃, and adding a binder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water) with the mass ratio of 6% of the composite powder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water is 4.5:2:1.5: 30); grinding and sieving (100 mesh), aging at 25 deg.C for 24 hr, tabletting, and isostatic pressing at 210MPa for 30 min; and (3) calcining the obtained sodium aluminum silicate/nano zinc oxide sheet at high temperature to obtain the ceramic, wherein the calcining temperature is 800 ℃, the heating rate is 7 ℃/min, and the heat preservation time is 3 h.
FIG. 2 is a graph showing the antibacterial effect of 1 wt% ZnO-doped sodium aluminum silicate (NAS/1.0Zn) ceramic prepared in example 2 on Streptococcus mutans.
The number of the NAS/1.0Zn ceramics obtained in the embodiment is obviously reduced compared with that of blank groups of bacteria, and the NAS/1.0Zn ceramics have certain antibacterial performance.
Example 3
Performing ball milling on sodium aluminum silicate and nano zinc oxide according to a mass ratio of 98% to 2% for 11 (adding absolute ethyl alcohol during ball milling, wherein the mass ratio of the composite powder to the absolute ethyl alcohol is 1:1.3) h, rotating at 450rpm, drying the slurry at 40 ℃, and adding a binder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water) accounting for 8% of the mass of the composite powder (the mass ratio of polyvinyl alcohol: glycerol: absolute ethyl alcohol: water is 5:2:1.5: 30); grinding and sieving (100 mesh), aging at 25 deg.C for 24 hr, tabletting, and isostatic pressing at 220MPa for 30 min; and (3) calcining the obtained sodium aluminum silicate/nano zinc oxide sheet at high temperature to obtain the ceramic, wherein the calcining temperature is 850 ℃, the heating rate is 8 ℃/min, and the heat preservation time is 3.5 h.
Example 4
Performing ball milling on sodium aluminum silicate and nano zinc oxide according to the mass ratio of 97% to 3% for 12 hours (adding absolute ethyl alcohol during ball milling, wherein the mass ratio of the composite powder to the absolute ethyl alcohol is 1:1.3), rotating at 450rpm, drying the slurry at 40 ℃, and adding a binder (polyvinyl alcohol: glycerol: absolute ethyl alcohol: water, wherein the mass ratio of the polyvinyl alcohol: glycerol: absolute ethyl alcohol: water is 5:2:1.5:30) accounting for 8% of the mass of the composite powder; grinding and sieving (100 mesh), aging at 25 deg.C for 24 hr, tabletting, and isostatic pressing at 220MPa for 30 min; and (3) calcining the obtained sodium aluminum silicate/nano zinc oxide sheet at high temperature to obtain the ceramic, wherein the calcining temperature is 800 ℃, the heating rate is 10 ℃/min, and the heat preservation time is 4 h.
FIG. 3 is a graph showing the antibacterial effect of sodium aluminum silicate (NAS/3.0Zn) ceramic doped with 3 wt% ZnO on Streptococcus mutans of example 4.
The NAS/3.0Zn ceramic obtained in the embodiment has a remarkably reduced number of bacteria compared with a blank group and kills all the bacteria, and shows that the NAS/3.0Zn ceramic has efficient antibacterial performance. Meanwhile, compared with the antibacterial effect of the NAS/1.0Zn ceramic on the streptococcus mutans of more than 80 percent, the NAS/3.0Zn ceramic has the antibacterial effect of 99 percent on the streptococcus mutans.
FIG. 4 is a statistical chart of the count of the antibacterial plates of the ceramics prepared in comparative example, example 2 and example 4.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (9)

1. A preparation method of a crown bridge repairing ceramic with efficient anti-deformation streptococcus is characterized by comprising the following steps: the method comprises the following steps:
(1) carrying out ball milling on sodium aluminum silicate and nano zinc oxide to obtain sodium aluminum silicate powder doped with nano zinc oxide; by mass percentage, 97 to 99.5 percent of sodium aluminum silicate and 0.5 to 3 percent of nano zinc oxide;
(2) mixing the sodium aluminum silicate powder doped with the nano zinc oxide with a binder uniformly, aging, granulating and molding to obtain molded sodium aluminum silicate/nano copper oxide;
(3) and calcining the formed sodium aluminum silicate/nano copper oxide to obtain the streptococcus mutans-resistant sodium aluminum silicate/nano copper oxide composite ceramic, namely the efficient streptococcus mutans-resistant crown and bridge repair ceramic.
2. The method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 1, wherein: the calcining conditions in the step (3) are as follows: the calcination temperature is 700 ℃ and 900 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 2-4 h.
3. The method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 1, wherein:
the dosage of the binder in the step (2) is 4-10% of the mass of the sodium aluminum silicate powder doped with the nano zinc oxide;
the binder consists of polyvinyl alcohol, glycerol and water; polyvinyl alcohol: glycerol: the mass ratio of water is (3-5): (1.5-2): 1.5: 30.
4. the method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 1, wherein: in the step (1), absolute ethyl alcohol is added into sodium aluminum silicate and nano zinc oxide during ball milling; the ball milling time is 8-12h, and the ball milling speed is 300-450 rpm.
5. The method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 1, wherein: after ball milling, drying, grinding and sieving treatment are carried out.
6. The method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 5, wherein: the drying temperature is 40-75 ℃; the mesh number of the sieve is 60-100 meshes.
7. The method for preparing the crown bridge repairing ceramic with the highly efficient anti-streptococcus mutans according to claim 1, wherein: the aging time in the step (2) is 20-30 h;
the molding is to adopt a hand-pulling type press to perform primary pressing to form a blank body for molding, and then perform secondary pressing through cold isostatic pressing, wherein the pressure is 200-220 MPa; the molding time is 25-35 min.
8. A crown bridge repair ceramic having high-potency streptococcus mutans resistance obtained by the production method according to any one of claims 1 to 7.
9. The use of the crown-bridge repair ceramic with highly potent anti-streptococcus mutans according to claim 8, wherein: the crown and bridge repairing ceramic with the efficient anti-deformation streptococcus is used for preparing a crown and bridge repairing material.
CN202210247626.7A 2022-03-14 2022-03-14 Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof Pending CN114712250A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894001A (en) * 2023-03-10 2023-04-04 湖南康纳新材料有限公司 High-hardness wear-resistant resin-permeable ceramic composite material and preparation method and application thereof

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CN108578250A (en) * 2018-05-07 2018-09-28 清华大学 A kind of resin penetration silicate composite material and its preparation and application
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CN109133885A (en) * 2018-09-18 2019-01-04 广东蓝狮医疗科技有限公司 A kind of preparation method of Zinc oxide doped antibacterial artificial hip joint ceramics bulb
CN109574664A (en) * 2018-12-14 2019-04-05 华南理工大学 It is a kind of efficiently to facilitate potassium-sodium niobate-based piezoelectricity implantation material of bone and the preparation method and application thereof
CN112960990A (en) * 2021-02-08 2021-06-15 同曦集团有限公司 Antibacterial, mildewproof and antiviral porous ceramic and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN107721420A (en) * 2017-09-06 2018-02-23 华南理工大学 A kind of cupric oxide doped potassium-sodium niobate antibacterial piezoelectric ceramics implant and its preparation and application
CN108578250A (en) * 2018-05-07 2018-09-28 清华大学 A kind of resin penetration silicate composite material and its preparation and application
CN109020513A (en) * 2018-09-18 2018-12-18 广东蓝狮医疗科技有限公司 A kind of preparation method of the aluminium oxide-zirconium oxide long acting antibiotic bioceramic of nano oxidized Copper-cladding Aluminum Bar
CN109133885A (en) * 2018-09-18 2019-01-04 广东蓝狮医疗科技有限公司 A kind of preparation method of Zinc oxide doped antibacterial artificial hip joint ceramics bulb
CN109574664A (en) * 2018-12-14 2019-04-05 华南理工大学 It is a kind of efficiently to facilitate potassium-sodium niobate-based piezoelectricity implantation material of bone and the preparation method and application thereof
CN112960990A (en) * 2021-02-08 2021-06-15 同曦集团有限公司 Antibacterial, mildewproof and antiviral porous ceramic and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894001A (en) * 2023-03-10 2023-04-04 湖南康纳新材料有限公司 High-hardness wear-resistant resin-permeable ceramic composite material and preparation method and application thereof

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Application publication date: 20220708