CN109133885A - A kind of preparation method of Zinc oxide doped antibacterial artificial hip joint ceramics bulb - Google Patents
A kind of preparation method of Zinc oxide doped antibacterial artificial hip joint ceramics bulb Download PDFInfo
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Abstract
The invention belongs to the technical fields of antibacterial implant material, disclose a kind of preparation method of the antibacterial artificial hip joint ceramics bulb of zinc doping.Method are as follows: by ball-milling medium, α-Al2O3, ZrO2(HfO2) and Y2O3Mixture, SiO2, ZnO, which is placed in ball-milling device, carries out ball milling, stirs drying, is granulated, cold isostatic compaction, and calcining, processing obtains Zinc oxide doped alurnina-zirconia ceramics bulb.And then antibacterial experiment has been carried out to the ceramic bulb of preparation using colony counting method, obtain good effect.Method of the invention is simple, and prepared implant has preferable antibacterial effect and mechanical property.
Description
Technical field
The preparation method of the present invention relates to a kind of artificial hip joint ceramics bulb with antibacterial action, in particular to it is a kind of
The preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide.
Background technique
Currently, the number injured with the aggravation of aging of population degree and due to participating in vigorous exercise is more and more, people
The demand in work joint is increasing, especially hip joint.According to incompletely statistics, the whole world needs replacing joint because of various diseases
Number be 4000 ~ 60,000,000, and annual joint replacement amount about 1,200,000 at present, differ greatly with actual demand.Face at present
The artificial hip joint that bed uses mainly has three kinds of metal material, ceramic material and high molecular material materials.Wherein, ceramic material is not
Only have the characteristics that high rigidity, high elastic modulus and high compression-strength and excellent wear resistance, but also has good
Biocompatibility and chemical stability, therefore be used to manufacture of intraocular hip joint and have been to be concerned by more and more people.
High purity aluminium oxide bioceramic has biologically inert, in human body and its stablizes, and hardness is high, is hardly worn,
It is commonly used for preparing artificial hip joint.But high purity aluminium oxide bioceramic belong to fragile material, bending strength and toughness compared with
It is low, brittle fracture is also easy to produce in use process.Zirconium oxide has been demonstrated to have preferable as toughener reinforced alumina ceramic
The fracture toughness and breaking strength of bioceramic material can be enhanced in effect.
On the other hand, during the implant surgery of biomaterial substitute, bacterium infection incidence is 5% ~ 10%, and is
The main reason for causing a disease and be lethal.Therefore, preparing a kind of biomaterial substitute with anti-microbial property can be reduced bacterium infection
Incidence, improve the success rate of implant surgery, to biomaterial application have important meaning.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of Zinc oxide doped antibacterial artificial hip joint ceramics bulb.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, comprising the following steps:
(1) ceramic bulb raw material (as mass fraction): 40% ~ 90% α-Al is weighed2O3, 8.0% ~ 59.9% ZrO2(HfO2) and
Y2O3Mixture, 0.1% ~ 1.0%SiO2, 0% ~ 1.0%ZnO；
(2) step (1) weighed ceramic powder is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and 6 ~ 12h of ball milling, the revolving speed of ball milling is 200 ~ 450rpm；
(3) by slurry obtained by step (2), heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 60 ~ 100 mesh；
(4) 1% ~ 8% bonding agent, regrinding sieving is added in grinding powder obtained by step (3)；
(5) ceramic powder obtained by step (4) is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, and pressure is 180 ~ 250MPa；
(6) sphere green body obtained by step (5) is dried to moisture content is 1% ~ 2%, and the sphere green body of drying is calcined；
(7) step (6) calcined sample is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
Preferably, slurry described in step (2) is made by ceramic powder material and dehydrated alcohol, solid content 50%.
Preferably, after drying described in step (3) moisture content of ceramic powder less than 0.5%.
Preferably, bonding agent described in step (4) is by polyethylene alcohol and water with (80% ~ 95%): the ratio of (5% ~ 20%)
It mixes.
Preferably, step (6) calcination temperature is 1450 ~ 1650 DEG C, and soaking time is 1 ~ 4h.
Preferably, the quality proportioning of step (7) bulb and water is 1:1.
Compared with prior art, the invention has the following advantages:
(1) used the present invention relates to a kind of high rigidity, the alurnina-zirconia ceramics bulb preparation method of high-wearing feature antibacterial
ZnO have antibacterial action, on the one hand can using dissolution zinc ion Zn2+Antibacterial, mechanism are that zinc oxide is thin by destroying
Bacterium cell membrane leads to the dissolution of cellular content, hinders the synthesis for being conducive to bacterial metabolism enzyme, destroys gene, thus
Bacterium is set to lose its biological activity etc. and complete sterilization process.On the other hand, the active oxygen antibacterial that zinc oxide generates, mechanism
It is found to be measured by electron spin resonance, zinc oxide can excite generation activity hydroxy, and activity hydroxy can be further by more
Step reaction generates H2O2Deng other active oxy groups.Active oxygen outstanding feature the most can exactly cause oxidative pressure, Ke Yizao
At the damage of DNA, cell membrane, protein, it might even be possible to cause cell death.Using method of the invention, diameter obtained is
The antibiotic rate of the alurnina-zirconia ceramics bulb of 28mm reaches 95%.
(2) there is better power using the Zinc oxide doped antibacterial artificial hip joint ceramics bulb of the method for the present invention preparation
Performance is learned, the zinc oxide of use is filled the ceramic material of micrometer structure, and the mechanical property of ceramic material can be improved；
(3) sintering temperature is reduced using the Zinc oxide doped antibacterial artificial hip joint ceramics bulb of the method for the present invention preparation,
Resource has been saved, and has been conducive to the raising of ceramic dense degree.
Detailed description of the invention
Fig. 1 is high rigidity, the alurnina-zirconia ceramics bulb preparation flow figure of high-wearing feature antibacterial.
Fig. 2 is the alurnina-zirconia ceramics ball schematic diagram of high rigidity, high-wearing feature antibacterial.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, but embodiments of the present invention are not limited to
This can refer to routine techniques progress for not specifically specified technological parameter.
α-Al in following embodiments2O3Raw material primary particle size d50It is 0.1 μm, purity 99.99%；ZrO2(HfO2) and
Y2O3Mixture material primary particle size d50It is 0.399 μm, purity 99.9%, ZnO is the common zinc oxide of market purchase.
Case study on implementation 1
A kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, comprising the following steps:
(1) ceramic bulb raw material (as mass fraction): 90% α-Al is weighed2O3, 9.75% ZrO2(HfO2) and Y2O3Mixing
Object, 0.25% SiO2；
(2) step (1) weighed ceramic powder is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and ball milling 8h, the revolving speed of ball milling is 250rpm；
(3) by slurry obtained by step (2), heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 80 mesh；
(4) 5% bonding agent, regrinding sieving is added in grinding powder obtained by step (3)；
(5) ceramic powder obtained by step (4) is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, pressure 240MPa；
(6) sphere green body obtained by step (5) is dried to moisture content is 1%, and the sphere green body of drying is calcined；
(7) step (6) calcined sample is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
Slurry described in step (2) is made by ceramic powder material and dehydrated alcohol, solid content 50%.
The moisture content of ceramic powder is less than 0.5% after drying described in step (3).
Bonding agent described in step (4) is to be mixed by polyethylene alcohol and water with the ratio of 80%:20%.
Step (6) calcination temperature is 1450 DEG C, soaking time 2h.
The quality proportioning of step (7) bulb and water is 1:1.
Case study on implementation 2
A kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, comprising the following steps:
(1) ceramic bulb raw material (as mass fraction): 90% α-Al is weighed2O3, 9.5% ZrO2(HfO2) and Y2O3Mixing
Object, 0.25% SiO2, 0.25% ZnO；
(2) step (1) weighed ceramic powder is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and ball milling 8h, the revolving speed of ball milling is 250rpm；
(3) by slurry obtained by step (2), heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 80 mesh；
(4) 5% bonding agent, regrinding sieving is added in grinding powder obtained by step (3)；
(5) ceramic powder obtained by step (4) is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, pressure 240MPa；
(6) sphere green body obtained by step (5) is dried to moisture content is 1%, and the sphere green body of drying is calcined；
(7) step (6) calcined sample is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
Slurry described in step (2) is made by ceramic powder material and dehydrated alcohol, solid content 50%.
The moisture content of ceramic powder is less than 0.5% after drying described in step (3).
Bonding agent described in step (4) is to be mixed by polyethylene alcohol and water with the ratio of 80%:20%.
Step (6) calcination temperature is 1550 DEG C, soaking time 2h.
The quality proportioning of step (7) bulb and water is 1:1.
Case study on implementation 3
A kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, comprising the following steps:
(1) ceramic bulb raw material (as mass fraction): 60% α-Al is weighed2O3, 39.2% ZrO2(HfO2) and Y2O3Mixing
Object, 0.4% SiO2, 0.4% ZnO；
(2) step (1) weighed ceramic powder is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and ball milling 8h, the revolving speed of ball milling is 250rpm；
(3) by slurry obtained by step (2), heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 80 mesh；
(4) 5% bonding agent, regrinding sieving is added in grinding powder obtained by step (3)；
(5) ceramic powder obtained by step (4) is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, pressure 240MPa；
(6) sphere green body obtained by step (5) is dried to moisture content is 1%, and the sphere green body of drying is calcined；
(7) step (6) calcined sample is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
Slurry described in step (2) is made by ceramic powder material and dehydrated alcohol, solid content 50%.
The moisture content of ceramic powder is less than 0.5% after drying described in step (3).
Bonding agent described in step (4) is to be mixed by polyethylene alcohol and water with the ratio of 80%:20%.
Step (6) calcination temperature is 1550 DEG C, soaking time 2h.
The quality proportioning of step (7) bulb and water is 1:1.
Case study on implementation 4
A kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, comprising the following steps:
(1) ceramic bulb raw material (as mass fraction): 50% α-Al is weighed2O3, 48.8% ZrO2(HfO2) and Y2O3Mixing
Object, 0.4% SiO2, 0.4% ZnO；
(2) step (1) weighed ceramic powder is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and ball milling 8h, the revolving speed of ball milling is 250rpm；
(3) by slurry obtained by step (2), heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 80 mesh；
(4) 5% bonding agent, regrinding sieving is added in grinding powder obtained by step (3)；
(5) ceramic powder obtained by step (4) is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, pressure 240MPa；
(6) sphere green body obtained by step (5) is dried to moisture content is 1%, and the sphere green body of drying is calcined；
(7) step (6) calcined sample is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
Slurry described in step (2) is made by ceramic powder material and dehydrated alcohol, solid content 50%.
The moisture content of ceramic powder is less than 0.5% after drying described in step (3).
Bonding agent described in step (4) is to be mixed by polyethylene alcohol and water with the ratio of 80%:20%.
Step (6) calcination temperature is 1550 DEG C, soaking time 2h.
The quality proportioning of step (7) bulb and water is 1:1.
While in order to verify the antibacterial effect of embodiment, specific antibacterial implementation and testing result are as follows:
(1) configuration and sterilizing of fluid nutrient medium
Using nutrient broth, proportion is meat soup 18g: distilled water or deionized water 1L, agitating and heating are boiled to complete
Dissolution, 121 DEG C of high-temperature sterilizations；
(2) configuration and sterilizing of solid medium
Solid medium proportion is: nutrient agar 33g: distilled water or deionized water 1L, agitating and heating are boiled to being completely dissolved,
After 121 DEG C of high-temperature sterilizations, being cooled to temperature is 50 DEG C -70 DEG C, and the height of solid medium is the 1/2-2/3 of culture dish height；
(3) purify and cultivate bacterium
The bacterium for taking 20 μ l to freeze draws 20 μ l after diluting 1000 times and is coated in (2) on agar plate, uses sterilizing pipette tips after cultivating 12h
The single bacterium colony selected, which is put into, to be filled shaking for 5ml fluid nutrient medium and cultivates 8-12h in tube；
(4) material and bacterium co-culture
A. it for suitable bacterial concentration in criterion calculation experiment and is configured with value=0.1 OD；
B. bacterium solution obtained in a is added to and is placed with alurnina-zirconia ceramics material (ceramics material prepared by embodiment 1 ~ 4
Material) orifice plate in co-culture 8h；
(5) coated plate
It is put in after being uniformly coated in the agar plate being cooled and shaped in (2) after bacterium solution in (4b) is diluted 100 times using spreading rod
12h is cultivated in 37 DEG C of biochemical cultivation cases；
(6) bacterium colony counts
It by culture, is bred by each single cells grown and forms macroscopic bacterium colony, count clump count, according to its dilution times
Number and sampling inoculum concentration, which can converse in sample, contains bacterium number.Culture dish of the clump count between 30-300 is selected to carry out bacterium colony meter
Number, then compares each material clump count, illustrates the anti-microbial property of material.The pottery of aluminium oxide-zirconium oxide prepared by embodiment 1 ~ 4
Shown in the anti-microbial property test result table 1 of ceramic material.
The anti-microbial property of the ceramic material of 1 case study on implementation of table preparation
In order to verify the mechanical property effect of embodiment, specific Mechanics Performance Testing scheme and testing result are as follows:
After tested ceramic material sanding and polishing, using the positive rectangular pyramid diamond penetrator that opposite face angle is 136 ° with
Load 9.807N(HV1) acts on material surface, after being kept for the stipulated time, measures impression catercorner length, then press formula
Calculate the size of hardness.The mechanical property of Zinc oxide doped antibacterial artificial hip joint ceramics bulb prepared by embodiment 1 ~ 4
Shown in the performance test results table 2.
The mechanical property of the ceramic material of 2 case study on implementation of table preparation
The above embodiment of the present invention is only intended to clearly illustrate the example that the present invention is lifted, and is not to implementation of the invention
The restriction of mode can also make other variations or changes in different ways, herein not on the basis of the field above description
It repeats one by one.Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in
Within the scope of protection of the claims of the present invention.
Claims (6)
1. a kind of preparation method of the antibacterial artificial hip joint ceramics bulb of doping zinc-oxide, which is characterized in that including following step
It is rapid:
S1. ceramic bulb raw material (as mass fraction): 40% ~ 90% α-Al is weighed2O3, 8.0% ~ 59.9% ZrO2(HfO2) and
Y2O3Mixture, 0.1% ~ 1.0%SiO2, 0% ~ 1.0%ZnO；
S2. the weighed ceramic powder of step S1 is put into 60 DEG C of drying, planetary ball mill is added in the ceramic powder after drying
In, it is made into slurry, and 6 ~ 12h of ball milling, the revolving speed of ball milling is 200 ~ 450rpm；
S3. by slurry obtained by step S2, heating stirring is dry at 70 DEG C, carries out being ground up, sieved processing, the mesh number of sieving
For 60 ~ 100 mesh；
S4. 1% ~ 8% bonding agent, regrinding sieving is added in grinding powder obtained by step S3；
S5. ceramic powder obtained by step S4 is still aging for 24 hours, green body is just pressed into using hand-pulling press, is used later
Cold isostatic compaction is suppressed again, and pressure is 180 ~ 250MPa；
S6. sphere green body obtained by step S5 is dried to moisture content is 1% ~ 2%, and the sphere green body of drying is calcined；
S7. the calcined sample of step S6 is placed in lathe process, obtained bulb is mixed to be put into grinder with water and be carried out
Polishing saves in drier after machine is dry out until ceramics spherical surface has bright gloss.
2. the preparation method of the antibacterial artificial hip joint ceramics bulb of a kind of doping zinc-oxide according to claim 1, special
Sign is that slurry described in step S2 is made by ceramic powder material and dehydrated alcohol, solid content 50%.
3. the preparation method of the antibacterial artificial hip joint ceramics bulb of a kind of doping zinc-oxide according to claim 1, special
Sign is that the moisture content of ceramic powder is less than 0.5% after drying described in step S3.
4. the preparation method of the antibacterial artificial hip joint ceramics bulb of a kind of doping zinc-oxide according to claim 1, special
Sign is that bonding agent described in step S4 is by polyethylene alcohol and water with (80% ~ 95%): the ratio of (5% ~ 20%) mixes.
5. the preparation method of the antibacterial artificial hip joint ceramics bulb of a kind of doping zinc-oxide according to claim 1, special
Sign is that calcination temperature described in step S6 is 1450 ~ 1650 DEG C, and soaking time is 1 ~ 4h.
6. the preparation method of the antibacterial artificial hip joint ceramics bulb of a kind of doping zinc-oxide according to claim 1, special
Sign is that the quality proportioning of bulb described in step S7 and water is 1:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114712250A (en) * | 2022-03-14 | 2022-07-08 | 华南理工大学 | Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof |
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| US3690062A (en) * | 1970-01-30 | 1972-09-12 | Suwa Seikosha Kk | Hard watch case |
| CN1063476A (en) * | 1991-01-24 | 1992-08-12 | 合肥工业大学 | Ceramic drawing die with precise structure and manufacture method thereof |
| CN103145448A (en) * | 2013-04-01 | 2013-06-12 | 漳州师范学院 | Technology for preparing antibacterial ceramic at low temperature |
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| CN114712250A (en) * | 2022-03-14 | 2022-07-08 | 华南理工大学 | Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof |
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