US20200199736A1 - Functional composite particles and the preparation method thereof - Google Patents
Functional composite particles and the preparation method thereof Download PDFInfo
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- US20200199736A1 US20200199736A1 US16/628,805 US201716628805A US2020199736A1 US 20200199736 A1 US20200199736 A1 US 20200199736A1 US 201716628805 A US201716628805 A US 201716628805A US 2020199736 A1 US2020199736 A1 US 2020199736A1
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- metallic particles
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- composite particle
- functional composite
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- 239000011246 composite particle Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013528 metallic particle Substances 0.000 claims abstract description 97
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 52
- 239000000919 ceramic Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 36
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- 238000009833 condensation Methods 0.000 claims description 16
- 230000000844 anti-bacterial effect Effects 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000004033 plastic Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- -1 AlTiN Inorganic materials 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 230000009471 action Effects 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 230000000845 anti-microbial effect Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002054 inoculum Substances 0.000 description 4
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- 239000002131 composite material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
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Images
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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Definitions
- the present invention relates to the technical field of composite materials, and in particular, to a functional composite particle and a preparation method thereof.
- Biocompatible ceramics not only have the mechanical compatibility and stability of ceramics, but also have affinity and biological activity with biological tissue, and can be applied in biological, medical, chemical, and other fields related to human body or animal body.
- single biocompatible ceramics have some limitations in practical application. For example, when the biocompatible ceramics are applied in artificial joints, it is easy to cause bacterial infections and, more seriously, local complications of bones may occur.
- the existing biocompatible ceramics can be further improved.
- one of the purposes of the present invention is to provide a functional composite particle and a preparation method thereof.
- the functional composite particle includes an inner core and a shell layer, wherein the inner core is consisted of functional metallic particles and has an outer surface, while the shell layer is a physical vapor deposition (PVD) ceramic layer consisted of biocompatible ceramic materials, and is attached to the outer surface of the inner core.
- the shell layer is a crystalline structure thereby allowing the ionic functional metallic particles to be sustained-released to the outside of the shell layer from the inner core via crystal boundaries.
- Another embodiment of the present invention provides a preparation method of the functional composite particle, comprising the following steps: by means of an evaporation-condensation process, putting a solid metal block composed of functional metallic particles into a crucible, and evaporating the solid metal block by heating to a vacuum PVD process furnace for condensation; and depositing a PVD ceramic layer composed of a biocompatible ceramic material on the outer surface of the functional metallic particles in the condensed state by means of a PVD process.
- Another embodiment of the present invention also provides an application of the functional composite particle.
- the functional composite particle is used for being coated on the surface of metal, cloth, ceramic, or plastic or implanted in metal, cloth, ceramic, or plastic.
- biocompatible ceramic materials are used to cover the outside surface of the functional metallic particles which have specific functions via the PVD process so as to form functional composite particles.
- this coating structure of the functional composite particle can prevent the functional metallic particles from being oxidized by ambient oxygen, and on the other hand, the ionic state of the functional metallic particles can be sustained-released through the crystal boundaries of the shell layer, such that the action time of the functional metallic particles can be prolonged.
- FIG. 1 shows a metallographic image of a functional composite particle according to an embodiment of the present invention
- FIG. 2 shows a metallographic image of another functional composite particle according to an embodiment of the present invention
- FIG. 3 shows an enlarged view of a portion of the metallographic image of the functional composite particle shown in FIG. 1 ;
- FIG. 4 shows a structure diagram of a functional composite particle according to an embodiment of the present invention.
- FIGS. 1 to 3 are metallographic images captured using an electron microscope, and the diagram in FIG. 4 is in a simplified form and adopts a non-precise scale and is only used for help to conveniently and clearly describe the embodiments of the present invention.
- FIG. 1 shows a metallographic image of a functional composite particle according to an embodiment of the present invention.
- FIG. 2 shows a metallographic image of another functional composite particle according to an embodiment of the present invention.
- FIG. 3 shows an enlarged view of a portion of the metallographic image of the functional composite particle shown in FIG. 1 .
- FIG. 4 shows a structure diagram of a functional composite particle according to an embodiment of the present invention.
- a functional composite particle 10 comprises an inner core 11 and a shell layer 12 .
- the inner core 11 is composed of functional metallic particles and has an outer surface 111 .
- the shell layer 12 is attached to the outer surface 111 of the inner core 11 and is a PVD ceramic layer consisting of a biocompatible ceramic material.
- the functional metallic particles of the inner core 11 have a particle diameter of 5 nm to 5 mm; and the shell layer 12 is a biocompatible ceramic layer consisting of a metal oxide or metal nitride composed of Zr, Ti, or Al, or a mixture of the metal oxide and the metal nitride, and has a thickness of 5 nm to 50000 nm, preferably 50 nm to 5000 nm, and surface hardness of 1000 HV to 4500 HV, preferably 3000 HV to 4000 HV.
- the shell layer 12 is a biocompatible ceramic layer consisting of ZrN, TiN, AlTiN, or Al 2 O 3 .
- the functional metallic particles of the inner core 11 are antibacterial metallic particles, which are Ag metallic particles, Zn metallic particles, Cu metallic particles, or a mixture thereof.
- the functional metallic particles of the inner core 11 are growth-promoting metallic particles, which are Ca metallic particles, K metallic particles, Mg metallic particles, or a mixture thereof.
- the shell layer 12 is of a crystalline structure and has a crystal boundary 121 which provides a passage leading to the outside of the shell layer 12 for the ionic state of the functional metallic particles in the inner core 11 .
- the functional metallic particles in the inner core 11 are sustained-released to the outside of the shell layer 12 through the crystal boundary 121 in the form of an ionic state.
- the shell layer 12 coated on the outer surface 111 of the inner core 11 can effectively prevent the functional metallic particles in the inner core 11 from contacting the ambient oxygen to avoid premature oxidation; and on the other hand, the functional metallic particles in the inner core 11 can also be sustained-released through the crystal boundary 121 of the shell layer 12 , such that the action time of the functional metallic particles are prolonged.
- the preparation method of the functional composite particl 10 shown in FIGS. 1 to 4 comprises the following steps:
- the particle diameter of the functional metallic particles after condensation is affected by the heating power of the heating source.
- the solid metal block composed of functional metallic particles is heated by using an electron gun as the heating source, wherein the current intensity of the electron gun is in a range of 60 A to 300 A, preferably 150 A to 250 A.
- the step of forming the PVD ceramic layer by means of a PVD process comprises: introducing nitrogen or oxygen with a purity of 99.999% into the vacuum PVD process furnace; at a bias voltage of 0 V to 1000 V, opening a target containing a biocompatible ceramic material, with an arc current of 120 A to 200 A; and depositing a PVD ceramic layer on the outer surface of the functional metallic particles in the condensed state by means of the PVD process.
- the shell layer 12 may be formed using a conventional PVD device by means of a conventional PVD process.
- the functional composite particles have different functions depending on the kind of the functional metallic particles.
- Ag metallic particles, Zn metallic particles, Cu metallic particles, or a mixture thereof correspond to antibacterial functional composite particles
- Ca metallic particles, K metallic particles, Mg metallic particles, or a mixture thereof correspond to growth-promoting functional composite particles.
- Functional composite particles can be further coated on the surface of metal, cloth (cotton, nonwoven fabric, etc.), ceramic, or plastic.
- the functional composite particles may be coated on the surface of a metal product, such as an orthopedic instrument, an artificial bone scaffold, or an artificial joint, to form an antibacterial coating or a growth-promoting coating, may be coated on the surface of a plastic product to form an antibacterial coating, and may also be coated on the surface of a nonwoven fabric to form an antibacterial coating, etc.
- the functional composite particles can also be implanted in metal, fabric, ceramic, or plastic to form a product having a specific function directly.
- an evaporation-condensation process By means of an evaporation-condensation process, putting a Mg metal block into a crucible, and evaporating the Mg metal block by heating with an electron gun at a current intensity of 200 A to a vacuum PVD process furnace for condensation; and introducing nitrogen with a purity of 99.999% into the vacuum PVD process furnace; at a bias voltage of 80 V to 100 V, opening a target containing a mixture of AlTi, with an arc current of 120 A to 200 A; and depositing an AlTiN ceramic layer on the outer surface of the Mg metallic particles in the condensed state by means of the PVD process, so as to form powder of AlTiN-Mg composite particles having a growth-promoting effect.
- the functional composite particles obtained in the above embodiments 1 and 2 were respectively coated on the surfaces of plastic articles as samples of the following antibacterial effect experiments. At the same time, another identical plastic article, the surface of which was not coated with the functional composite material, was taken as a control. Test method: please refer to ISO22196:2011.
- the values of the antimicrobial activity in the tables are the values of the antimicrobial activity of the samples with respect to the controls.
- the biocompatible ceramic material is coated on the outer surface of functional metallic particles having a specific function by means of the PVD process to form a functional composite particle.
- the ionic state of the functional metallic particles in the functional composite particle can be sustained-released through the crystal boundaries of the shell layer, such that the action time of the functional metallic particles can be prolonged.
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CN110238387A (zh) * | 2019-06-25 | 2019-09-17 | 纳狮新材料(浙江)有限公司 | 功能复合粒子及其制备方法 |
CN112872351B (zh) * | 2021-01-13 | 2023-07-14 | 太原理工大学 | 一种混杂协同增强铁基耐磨材料的制备方法 |
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CN111295475A (zh) | 2020-06-16 |
CN111295475B (zh) | 2022-07-26 |
WO2019014854A1 (fr) | 2019-01-24 |
EP3656488A4 (fr) | 2021-01-06 |
CN111491751B (zh) | 2022-07-26 |
EP3656913A1 (fr) | 2020-05-27 |
WO2019015621A1 (fr) | 2019-01-24 |
JP6900570B2 (ja) | 2021-07-07 |
CN111491751A (zh) | 2020-08-04 |
JP2020531680A (ja) | 2020-11-05 |
EP3656488A1 (fr) | 2020-05-27 |
US20210156081A1 (en) | 2021-05-27 |
JP2020526682A (ja) | 2020-08-31 |
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JP7122368B2 (ja) | 2022-08-19 |
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