CN116947514B - Antibacterial ceramic material and preparation process thereof - Google Patents
Antibacterial ceramic material and preparation process thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 84
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 71
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 50
- 239000001110 calcium chloride Substances 0.000 claims abstract description 45
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 45
- -1 calcium nitride Chemical class 0.000 claims abstract description 38
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 38
- 239000011575 calcium Substances 0.000 claims abstract description 33
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 33
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 33
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 33
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000003381 stabilizer Substances 0.000 claims abstract description 24
- 239000004927 clay Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011268 mixed slurry Substances 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000005056 compaction Methods 0.000 claims abstract description 3
- 238000010025 steaming Methods 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 47
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 47
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 29
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 26
- 239000012745 toughening agent Substances 0.000 claims description 26
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 21
- 229940075613 gadolinium oxide Drugs 0.000 claims description 21
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 21
- 239000011787 zinc oxide Substances 0.000 claims description 21
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 18
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 16
- 239000000022 bacteriostatic agent Substances 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 230000000845 anti-microbial effect Effects 0.000 claims 8
- 239000004599 antimicrobial Substances 0.000 claims 8
- 238000013329 compounding Methods 0.000 description 12
- 239000003242 anti bacterial agent Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 230000007613 environmental effect Effects 0.000 description 10
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 8
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 235000010755 mineral Nutrition 0.000 description 5
- 238000002390 rotary evaporation Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910001626 barium chloride Inorganic materials 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000011698 potassium fluoride Substances 0.000 description 4
- 235000003270 potassium fluoride Nutrition 0.000 description 4
- 230000003385 bacteriostatic effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000009918 complex formation Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of ceramic materials, and particularly discloses an antibacterial ceramic material and a preparation process thereof. An antibacterial ceramic material comprising the following components: alumina, clay, stabilizer, fluxing agent, bacteriostat and flexibilizer, wherein the flexibilizer is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride. The preparation process comprises the following steps: step 1), weighing the raw materials in proportion, and adding water to mix to obtain mixed slurry; step 2), rotary steaming and concentrating the mixed slurry to obtain mud cakes; step 3), drying the mud cake to obtain a blank; and 4) placing the blank into a mould for compaction, heating to 900-1000 ℃, keeping the temperature for 15-30min, heating to 1300-1350 ℃, keeping the temperature for 60-90min, heating to 1450-1500 ℃, keeping the temperature for 60-90min, cooling to room temperature at a speed of 1.2-1.4 ℃/min, and demoulding to obtain the antibacterial ceramic material. The invention has the advantage of improving the toughness of the alumina ceramic material.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to an antibacterial ceramic material and a preparation process thereof.
Background
The alumina ceramic is ceramic prepared by taking alumina as a main raw material, has the advantages of high melting point, high hardness, high wear resistance and the like, has hardness inferior to that of diamond, has smooth surface and small friction coefficient, and is particularly suitable for wear-resistant materials in high-temperature environments.
With the development of material application, the demand for ceramic materials is increased, and the antibacterial ceramic is a novel material developed on the premise that the ceramic materials are required to have antibacterial and bacteriostatic properties, and the ceramic materials have antibacterial properties by adding antibacterial components, so that the application range of the ceramic materials is expanded.
However, although the alumina ceramic material has high hardness, it has high brittleness, and is liable to crack and break, which affects the service life of the ceramic material, and there is room for improvement.
Disclosure of Invention
In order to improve the toughness of an alumina ceramic material, the application provides an antibacterial ceramic material and a preparation process thereof.
In a first aspect, the present application provides an antibacterial ceramic material, which adopts the following technical scheme:
an antibacterial ceramic material comprises the following components in parts by mass:
93-95 parts of aluminum oxide;
2-4 parts of clay;
0.4-0.6 part of stabilizer;
0.8-1.2 parts of fluxing agent;
0.4-0.6 part of bacteriostat;
0.9-1.1 parts of toughening agent;
the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride.
Through adopting above-mentioned technical scheme, through adding the toughener that adopts calcium chloride, potassium sulfate, sodium carbonate, calcium nitride complex formation, at refrigerated in-process, under potassium sulfate, sodium carbonate, calcium nitride's effect, calcium chloride can crystallize and form the calcium chloride whisker to make in the ceramic material by the calcium chloride whisker filling, thereby greatly increased ceramic material's toughness, make ceramic material be difficult for appearing crackle and fracture, life is longer, application scope is wider.
By adding the stabilizer, the ceramic material has better human stability and wear resistance.
The addition of the fluxing agent enables the sintering temperature to be lower, the sintering is not required to be carried out at an excessive temperature, the toughening agent can form calcium chloride whisker at a proper sintering temperature, and the toughening effect is good.
By adding the bacteriostat, the ceramic material has better antibacterial and bacteriostatic effects, so that the application range of the ceramic material is wider.
Preferably, the mass ratio of the calcium chloride, the potassium sulfate, the sodium carbonate and the calcium nitride is 8.9-9.1:2.9-3.1:0.9-1.1:1.9-2.1.
By adopting the technical scheme, the calcium chloride whisker has better effect by specifically selecting the mass proportion range of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the toughness of the ceramic material is better improved, so that the ceramic material is less prone to damage such as cracks, breakage and the like.
Preferably, the mass ratio of the alumina, the clay, the stabilizer, the fluxing agent, the bacteriostatic agent and the toughening agent is as follows: 94:3:0.5:1:0.5:1.
by adopting the technical scheme, the calcium chloride whisker can be better formed by specifically selecting the mass ratio of the calcium chloride, the potassium sulfate, the sodium carbonate and the calcium nitride, and the toughening ceramic material has better effect.
Preferably, the stabilizer is a compound of gadolinium oxide, yttrium oxide and lanthanum oxide.
By adopting the technical scheme, the thermal stability and the wear resistance of the ceramic material can be better improved by specifically selecting gadolinium oxide, yttrium oxide and lanthanum oxide to be compounded as the stabilizer.
Preferably, the mass ratio of gadolinium oxide to yttrium oxide to lanthanum oxide is 0.9-1.1:2.9-3.1:1.9-2.1.
By adopting the technical scheme, the effect of improving the wear resistance of the ceramic material is better by specifically selecting the mass ratio of gadolinium oxide, yttrium oxide and lanthanum oxide.
Preferably, the fluxing agent is a compound of zirconium oxide and titanium oxide.
By adopting the technical scheme, the zirconia and the titanium oxide are specifically selected to be compounded to serve as fluxing agents, so that the sintering temperature is better reduced, the energy consumption is reduced, and the process difficulty is reduced.
Preferably, the mass ratio of the zirconia to the titania is 2.9-3.1:1.9-2.1.
By adopting the technical scheme, the raw materials are easier to melt by specifically selecting the mass ratio of the zirconia to the titania, so that the sintering process is simpler, the required processing temperature of the toughening agent can be matched better, the calcium chloride whisker can be formed better, and the toughening effect is better.
Preferably, the bacteriostatic agent is a compound of zinc oxide and silver ion bacteriostatic agent.
By adopting the technical scheme, the bacteriostatic agent is formed by compounding the zinc oxide and the silver ion bacteriostatic agent, so that the bacteriostatic effect is better.
Preferably, the mass ratio of the zinc oxide to the silver ion bacteriostat is 0.9-1.1:1.9-2.1.
By adopting the technical scheme, the antibacterial effect of the ceramic material is further improved by specifically selecting the mass ratio of the zinc oxide and the silver ion antibacterial agent, and the application range of the ceramic material is better widened.
In a second aspect, the present application provides a preparation process of an antibacterial ceramic material, which adopts the following technical scheme:
step 1), weighing the raw materials in proportion, and adding water to mix to obtain mixed slurry;
step 2), rotary steaming and concentrating the mixed slurry to obtain mud cakes;
step 3), drying the mud cake to obtain a blank;
and 4) placing the blank into a mould for compaction, heating to 900-1000 ℃, keeping the temperature for 15-30min, heating to 1300-1350 ℃, keeping the temperature for 60-90min, heating to 1450-1500 ℃, keeping the temperature for 60-90min, cooling to room temperature at a speed of 1.2-1.4 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Through adopting above-mentioned technical scheme, through the segmentation heating, avoid quick heating to lead to the fracture phenomenon, through cooling with special speed for calcium chloride cooling solidification's in-process can form a large amount of calcium chloride whisker under the cooperation of potassium sulfate, sodium carbonate, calcium nitride, thereby pack in ceramic material, and then make ceramic material's toughness improve by a wide margin.
In summary, the present application has the following beneficial effects:
1. because this application adopts calcium chloride, potassium sulfate, sodium carbonate, the toughener that calcium nitride compound formed through adding, at refrigerated in-process, under potassium sulfate, sodium carbonate, calcium nitride's effect, calcium chloride can crystallize and form the calcium chloride whisker to make in the ceramic material by the calcium chloride whisker packing, thereby greatly increased ceramic material's toughness, make ceramic material be difficult for appearing crackle and fracture, life is longer, application scope is wider.
2. In the application, the mass proportion range of the calcium chloride, the potassium sulfate, the sodium carbonate and the calcium nitride is preferably selected, so that the effect of forming the calcium chloride whisker is better, the toughness of the ceramic material is better improved, and the ceramic material is less prone to damage such as cracks and breakage.
3. The ceramic material is preferably heated in a segmented manner, so that cracking caused by rapid heating is avoided, and the temperature is reduced at a special speed, so that a large number of calcium chloride whiskers can be formed under the synergistic cooperation of potassium sulfate, sodium carbonate and calcium nitride in the process of cooling and solidifying the calcium chloride, and the ceramic material is filled with the ceramic material, so that the toughness of the ceramic material is greatly improved.
Detailed Description
The present application is described in further detail below with reference to examples.
Example 1
An antibacterial ceramic material is prepared from alumina, clay, stabilizer, flux, antibacterial agent and toughening agent.
Wherein, the alumina is purchased from the company of Boyi Cheng Jialv, 325 mesh, CAS number: 1344-28-1, and the content is 99 percent.
Among them, clay is purchased from Shijia's cymbaze mineral products limited company, 325 mesh.
Wherein the stabilizer is the combination of gadolinium oxide, yttrium oxide and lanthanum oxide, and the mass ratio of the gadolinium oxide to the yttrium oxide to the lanthanum oxide is 0.9:2.9:1.9.
gadolinium oxide is purchased from Jinbang environmental protection technology, inc., CAS number: 12064-62-9, and the content is 99%.
Yttria was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-36-9, and the content is 99%.
Lanthanum oxide was purchased from zheng state raw and chemical products limited, CAS number: 1312-81-8, content 99%.
Wherein, the fluxing agent is the compounding of zirconia and titanium oxide, and the mass ratio of the zirconia to the titanium oxide is 2.9:1.9.
zirconia was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-23-4, and the content is 99.8 percent.
Titanium oxide was purchased from Xuancheng Jinrui New Material Co., ltd., CAS number: 13463-67-7, and the content is 99.5 percent.
Wherein the bacteriostat is the compounding of zinc oxide and silver ion bacteriostat, and the mass ratio of the zinc oxide to the silver ion bacteriostat is 0.9:1.9.
zinc oxide was purchased from Shandong Wang Tongxi chemical Co., ltd., CAS number: 1314-13-2, content 99.7%.
Silver ion bacteriostat is purchased from Nanjing Tianshi blue shield biotechnology limited company, model: LD940, inorganic nano silver antibacterial agent, 98%.
Wherein the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 8.9:2.9:0.9:1.9.
calcium chloride was purchased from wuhan's biotechnology limited, CAS number: 10043-52-4, and the content is 99%.
Potassium sulfate was purchased from Hubei Xingzhou science and technology Co., ltd., CAS number: 7778-80-5, and the content is 99%.
Sodium carbonate was purchased from Jinbang environmental protection technology Co., ltd., CAS number: 497-19-8, and the content is 99%.
Calcium nitride was purchased from Shanghai Bike New Material technologies Co., ltd., CAS number: 12013-82-0, and the content is 99.5%.
The preparation process of the antibacterial ceramic material comprises the following steps:
step 1), 93kg of alumina, 2kg of clay, 0.4kg of stabilizer, 0.8kg of fluxing agent, 0.4kg of bacteriostatic agent, 0.9kg of toughening agent and 50kg of water are weighed and put into a stirring kettle, the rotating speed is 60r/min, stirring is carried out for 3min,2500r/min, homogenizing is carried out for 5min, and the mixed slurry is obtained.
And 2) carrying out rotary evaporation concentration on the mixed slurry, wherein the pressure is 0.01MPa, the concentration temperature is 60 ℃, and the mud cake with the water content of about 15% is obtained.
And 3) naturally drying the mud cake to obtain a blank with the water content lower than 2%.
And 4) placing the blank into a mould, compacting, placing the mould into an electric furnace, heating to 900 ℃, keeping the temperature for 30min, then heating to 1300 ℃, keeping the temperature for 90min, then heating to 1450 ℃, keeping the temperature for 90min, then cooling to room temperature at a speed of 1.2 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Example 2
An antibacterial ceramic material is prepared from alumina, clay, stabilizer, flux, antibacterial agent and toughening agent.
Wherein, the alumina is purchased from the company of Boyi Cheng Jialv, 325 mesh, CAS number: 1344-28-1, and the content is 99 percent.
Among them, clay is purchased from Shijia's cymbaze mineral products limited company, 325 mesh.
Wherein the stabilizer is the combination of gadolinium oxide, yttrium oxide and lanthanum oxide, and the mass ratio of the gadolinium oxide to the yttrium oxide to the lanthanum oxide is 1:3:2.
gadolinium oxide is purchased from Jinbang environmental protection technology, inc., CAS number: 12064-62-9, and the content is 99%.
Yttria was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-36-9, and the content is 99%.
Lanthanum oxide was purchased from zheng state raw and chemical products limited, CAS number: 1312-81-8, content 99%.
Wherein the fluxing agent is the compounding of zirconia and titanium oxide, and the mass ratio of the zirconia to the titanium oxide is 3:2.
zirconia was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-23-4, and the content is 99.8 percent.
Titanium oxide was purchased from Xuancheng Jinrui New Material Co., ltd., CAS number: 13463-67-7, and the content is 99.5 percent.
Wherein the bacteriostat is the compounding of zinc oxide and silver ion bacteriostat, and the mass ratio of the zinc oxide to the silver ion bacteriostat is 1:2.
zinc oxide was purchased from Shandong Wang Tongxi chemical Co., ltd., CAS number: 1314-13-2, content 99.7%.
Silver ion bacteriostat is purchased from Nanjing Tianshi blue shield biotechnology limited company, model: LD940, inorganic nano silver antibacterial agent, 98%.
Wherein the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 9:3:1:2.
calcium chloride was purchased from wuhan's biotechnology limited, CAS number: 10043-52-4, and the content is 99%.
Potassium sulfate was purchased from Hubei Xingzhou science and technology Co., ltd., CAS number: 7778-80-5, and the content is 99%.
Sodium carbonate was purchased from Jinbang environmental protection technology Co., ltd., CAS number: 497-19-8, and the content is 99%.
Calcium nitride was purchased from Shanghai Bike New Material technologies Co., ltd., CAS number: 12013-82-0, and the content is 99.5%.
The preparation process of the antibacterial ceramic material comprises the following steps:
step 1), 94kg of alumina, 3kg of clay, 0.5kg of stabilizer, 1kg of fluxing agent, 0.5kg of bacteriostat, 1kg of toughening agent and 50kg of water are weighed and put into a stirring kettle, the rotating speed is 60r/min, stirring is carried out for 3min,2500r/min, homogenizing is carried out for 5min, and the mixed slurry is obtained.
And 2) carrying out rotary evaporation concentration on the mixed slurry, wherein the pressure is 0.01MPa, the concentration temperature is 60 ℃, and the mud cake with the water content of about 15% is obtained.
And 3) naturally drying the mud cake to obtain a blank with the water content lower than 2%.
And 4) placing the blank into a mould, compacting, placing the mould into an electric furnace, heating to 900 ℃, keeping the temperature for 30min, then heating to 1300 ℃, keeping the temperature for 90min, then heating to 1450 ℃, keeping the temperature for 90min, then cooling to room temperature at a speed of 1.2 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Example 3
An antibacterial ceramic material is prepared from alumina, clay, stabilizer, flux, antibacterial agent and toughening agent.
Wherein, the alumina is purchased from the company of Boyi Cheng Jialv, 325 mesh, CAS number: 1344-28-1, and the content is 99 percent.
Among them, clay is purchased from Shijia's cymbaze mineral products limited company, 325 mesh.
Wherein the stabilizer is the combination of gadolinium oxide, yttrium oxide and lanthanum oxide, and the mass ratio of the gadolinium oxide to the yttrium oxide to the lanthanum oxide is 1:3:2.
gadolinium oxide is purchased from Jinbang environmental protection technology, inc., CAS number: 12064-62-9, and the content is 99%.
Yttria was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-36-9, and the content is 99%.
Lanthanum oxide was purchased from zheng state raw and chemical products limited, CAS number: 1312-81-8, content 99%.
Wherein the fluxing agent is the compounding of zirconia and titanium oxide, and the mass ratio of the zirconia to the titanium oxide is 3:2.
zirconia was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-23-4, and the content is 99.8 percent.
Titanium oxide was purchased from Xuancheng Jinrui New Material Co., ltd., CAS number: 13463-67-7, and the content is 99.5 percent.
Wherein the bacteriostat is the compounding of zinc oxide and silver ion bacteriostat, and the mass ratio of the zinc oxide to the silver ion bacteriostat is 1:2.
zinc oxide was purchased from Shandong Wang Tongxi chemical Co., ltd., CAS number: 1314-13-2, content 99.7%.
Silver ion bacteriostat is purchased from Nanjing Tianshi blue shield biotechnology limited company, model: LD940, inorganic nano silver antibacterial agent, 98%.
Wherein the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 9:3:1:2.
calcium chloride was purchased from wuhan's biotechnology limited, CAS number: 10043-52-4, and the content is 99%.
Potassium sulfate was purchased from Hubei Xingzhou science and technology Co., ltd., CAS number: 7778-80-5, and the content is 99%.
Sodium carbonate was purchased from Jinbang environmental protection technology Co., ltd., CAS number: 497-19-8, and the content is 99%.
Calcium nitride was purchased from Shanghai Bike New Material technologies Co., ltd., CAS number: 12013-82-0, and the content is 99.5%.
The preparation process of the antibacterial ceramic material comprises the following steps:
step 1), 94kg of alumina, 3kg of clay, 0.5kg of stabilizer, 1kg of fluxing agent, 0.5kg of bacteriostat, 1kg of toughening agent and 50kg of water are weighed and put into a stirring kettle, the rotating speed is 60r/min, stirring is carried out for 3min,2500r/min, homogenizing is carried out for 5min, and the mixed slurry is obtained.
And 2) carrying out rotary evaporation concentration on the mixed slurry, wherein the pressure is 0.01MPa, the concentration temperature is 60 ℃, and the mud cake with the water content of about 15% is obtained.
And 3) naturally drying the mud cake to obtain a blank with the water content lower than 2%.
And 4) placing the blank into a mould, compacting, placing the mould into an electric furnace, heating to 950 ℃, keeping the temperature for 20min, then heating to 1325 ℃, keeping the temperature for 75min, then heating to 1475 ℃, keeping the temperature for 75min, then cooling to room temperature at a speed of 1.3 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Example 4
An antibacterial ceramic material is prepared from alumina, clay, stabilizer, flux, antibacterial agent and toughening agent.
Wherein, the alumina is purchased from the company of Boyi Cheng Jialv, 325 mesh, CAS number: 1344-28-1, and the content is 99 percent.
Among them, clay is purchased from Shijia's cymbaze mineral products limited company, 325 mesh.
Wherein the stabilizer is the combination of gadolinium oxide, yttrium oxide and lanthanum oxide, and the mass ratio of the gadolinium oxide to the yttrium oxide to the lanthanum oxide is 1:3:2.
gadolinium oxide is purchased from Jinbang environmental protection technology, inc., CAS number: 12064-62-9, and the content is 99%.
Yttria was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-36-9, and the content is 99%.
Lanthanum oxide was purchased from zheng state raw and chemical products limited, CAS number: 1312-81-8, content 99%.
Wherein the fluxing agent is the compounding of zirconia and titanium oxide, and the mass ratio of the zirconia to the titanium oxide is 3:2.
zirconia was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-23-4, and the content is 99.8 percent.
Titanium oxide was purchased from Xuancheng Jinrui New Material Co., ltd., CAS number: 13463-67-7, and the content is 99.5 percent.
Wherein the bacteriostat is the compounding of zinc oxide and silver ion bacteriostat, and the mass ratio of the zinc oxide to the silver ion bacteriostat is 1:2.
zinc oxide was purchased from Shandong Wang Tongxi chemical Co., ltd., CAS number: 1314-13-2, content 99.7%.
Silver ion bacteriostat is purchased from Nanjing Tianshi blue shield biotechnology limited company, model: LD940, inorganic nano silver antibacterial agent, 98%.
Wherein the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 9:3:1:2.
calcium chloride was purchased from wuhan's biotechnology limited, CAS number: 10043-52-4, and the content is 99%.
Potassium sulfate was purchased from Hubei Xingzhou science and technology Co., ltd., CAS number: 7778-80-5, and the content is 99%.
Sodium carbonate was purchased from Jinbang environmental protection technology Co., ltd., CAS number: 497-19-8, and the content is 99%.
Calcium nitride was purchased from Shanghai Bike New Material technologies Co., ltd., CAS number: 12013-82-0, and the content is 99.5%.
The preparation process of the antibacterial ceramic material comprises the following steps:
step 1), 94kg of alumina, 3kg of clay, 0.5kg of stabilizer, 1kg of fluxing agent, 0.5kg of bacteriostat, 1kg of toughening agent and 50kg of water are weighed and put into a stirring kettle, the rotating speed is 60r/min, stirring is carried out for 3min,2500r/min, homogenizing is carried out for 5min, and the mixed slurry is obtained.
And 2) carrying out rotary evaporation concentration on the mixed slurry, wherein the pressure is 0.01MPa, the concentration temperature is 60 ℃, and the mud cake with the water content of about 15% is obtained.
And 3) naturally drying the mud cake to obtain a blank with the water content lower than 2%.
And 4) placing the blank into a mould, compacting, placing the mould into an electric furnace, heating to 1000 ℃, keeping the temperature for 15min, then heating to 1350 ℃, keeping the temperature for 60min, then heating to 1500 ℃, keeping the temperature for 60min, then cooling to room temperature at a speed of 1.4 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Example 5
An antibacterial ceramic material is prepared from alumina, clay, stabilizer, flux, antibacterial agent and toughening agent.
Wherein, the alumina is purchased from the company of Boyi Cheng Jialv, 325 mesh, CAS number: 1344-28-1, and the content is 99 percent.
Among them, clay is purchased from Shijia's cymbaze mineral products limited company, 325 mesh.
Wherein the stabilizer is the compounding of gadolinium oxide, yttrium oxide and lanthanum oxide, and the mass ratio of the gadolinium oxide to the yttrium oxide to the lanthanum oxide is 1.1:3.1:2.1.
gadolinium oxide is purchased from Jinbang environmental protection technology, inc., CAS number: 12064-62-9, and the content is 99%.
Yttria was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-36-9, and the content is 99%.
Lanthanum oxide was purchased from zheng state raw and chemical products limited, CAS number: 1312-81-8, content 99%.
Wherein, the fluxing agent is the compounding of zirconia and titanium oxide, and the mass ratio of the zirconia to the titanium oxide is 3.1:2.1.
zirconia was purchased from Shandong Hao chemical Co., ltd., CAS number: 1314-23-4, and the content is 99.8 percent.
Titanium oxide was purchased from Xuancheng Jinrui New Material Co., ltd., CAS number: 13463-67-7, and the content is 99.5 percent.
Wherein the bacteriostat is the compounding of zinc oxide and silver ion bacteriostat, and the mass ratio of the zinc oxide to the silver ion bacteriostat is 1.1:2.1.
zinc oxide was purchased from Shandong Wang Tongxi chemical Co., ltd., CAS number: 1314-13-2, content 99.7%.
Silver ion bacteriostat is purchased from Nanjing Tianshi blue shield biotechnology limited company, model: LD940, inorganic nano silver antibacterial agent, 98%.
Wherein the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride, and the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 9.1:3.1:1.1:2.1.
calcium chloride was purchased from wuhan's biotechnology limited, CAS number: 10043-52-4, and the content is 99%.
Potassium sulfate was purchased from Hubei Xingzhou science and technology Co., ltd., CAS number: 7778-80-5, and the content is 99%.
Sodium carbonate was purchased from Jinbang environmental protection technology Co., ltd., CAS number: 497-19-8, and the content is 99%.
Calcium nitride was purchased from Shanghai Bike New Material technologies Co., ltd., CAS number: 12013-82-0, and the content is 99.5%.
The preparation process of the antibacterial ceramic material comprises the following steps:
step 1), weighing 95kg of alumina, 4kg of clay, 0.6kg of stabilizer, 1.2kg of fluxing agent, 0.6kg of bacteriostatic agent, 1.1kg of toughening agent and 50kg of water, putting into a stirring kettle, stirring for 3min at the rotating speed of 60r/min, stirring for 2500r/min, homogenizing for 5min, and uniformly mixing to obtain mixed slurry.
And 2) carrying out rotary evaporation concentration on the mixed slurry, wherein the pressure is 0.01MPa, the concentration temperature is 60 ℃, and the mud cake with the water content of about 15% is obtained.
And 3) naturally drying the mud cake to obtain a blank with the water content lower than 2%.
And 4) placing the blank into a mould, compacting, placing the mould into an electric furnace, heating to 1000 ℃, keeping the temperature for 15min, then heating to 1350 ℃, keeping the temperature for 60min, then heating to 1500 ℃, keeping the temperature for 60min, then cooling to room temperature at a speed of 1.4 ℃/min, and demoulding to obtain the antibacterial ceramic material.
Comparative example 1
An antibacterial ceramic material, compared with example 3, differs only in that:
the calcium chloride is replaced by the same amount of calcium oxide.
Wherein, the calcium oxide is from commercial market, CAS number: 1305-78-8, and the content is 99%.
Comparative example 2
An antibacterial ceramic material, compared with example 3, differs only in that:
potassium fluoride is used to replace potassium sulfate in equal amount.
Wherein, potassium fluoride is from commercial market, CAS number: 7789-23-9, content 99%.
Comparative example 3
An antibacterial ceramic material, compared with example 3, differs only in that:
barium chloride was used in place of sodium carbonate in equal amounts.
Wherein, barium chloride is from commercial, CAS number: 10361-37-2, content 99%.
Comparative example 4
An antibacterial ceramic material, compared with example 3, differs only in that:
the equivalent replacement of calcium nitride with calcium sulfide.
Wherein, the calcium sulfide is from commercial market, CAS number: 20548-54-3 and the content is 99 percent.
Comparative example 5
An antibacterial ceramic material, compared with example 3, differs only in that:
the calcium chloride is replaced by the same amount of calcium oxide.
Potassium fluoride is used to replace potassium sulfate in equal amount.
Barium chloride was used in place of sodium carbonate in equal amounts.
The equivalent replacement of calcium nitride with calcium sulfide.
Wherein, the calcium oxide is from commercial market, CAS number: 1305-78-8, and the content is 99%.
Wherein, potassium fluoride is from commercial market, CAS number: 7789-23-9, content 99%.
Wherein, barium chloride is from commercial, CAS number: 10361-37-2, content 99%.
Wherein, the calcium sulfide is from commercial market, CAS number: 20548-54-3 and the content is 99 percent.
Comparative example 6
An antibacterial ceramic material, compared with example 3, differs only in that:
in step 4), the temperature is reduced to room temperature at a speed of 2 ℃/min.
Comparative example 7
An antibacterial ceramic material, compared with example 3, differs only in that:
in step 4), the temperature is reduced to room temperature at a speed of 1 ℃/min.
Experiment 1
The fracture toughness values of the samples prepared from the antibacterial ceramic materials of each example and comparative example were tested according to GB/T23806-2009 method for fine ceramic fracture toughness test method Single side Pre-crack Beam (SEPB) method.
The test was performed using a three-point bending apparatus, and sample I was used as the sample specification.
Experiment 2
The antibacterial rate of the samples prepared from the antibacterial ceramic materials of each example and comparative example was examined according to JC/T897-2002 antibacterial ceramic product antibacterial Property.
The specific test data for experiments 1-2 are detailed in Table 1.
TABLE 1
According to the data comparison of table 1, when calcium chloride, potassium sulfate, sodium carbonate and calcium nitride are adopted as toughening agents (examples 1-3), the fracture toughness value of the ceramic material is obviously improved compared with each comparative example, and the ceramic material has higher toughness, is not easy to crack and break, has longer service life and is not easy to damage, and when any one or all of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride is replaced by other materials, whiskers cannot be formed in the ceramic material, no obvious toughening effect exists, and the toughness of the ceramic material is only a conventional value.
Compared with comparative examples 6-7, the specific cooling speed is selected after sintering to facilitate the formation of calcium chloride whisker, and the toughening effect is improved more obviously.
By adding the bacteriostat, the ceramic material has better bacteriostasis performance, wider application range and better quality.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. An antimicrobial ceramic material, characterized in that: comprises the following components in parts by mass:
93-95 parts of aluminum oxide;
2-4 parts of clay;
0.4-0.6 part of stabilizer;
0.8-1.2 parts of fluxing agent;
0.4-0.6 part of bacteriostat;
0.9-1.1 parts of toughening agent;
the toughening agent is a compound of calcium chloride, potassium sulfate, sodium carbonate and calcium nitride;
the mass ratio of the calcium chloride to the potassium sulfate to the sodium carbonate to the calcium nitride is 8.9-9.1:2.9-3.1:0.9-1.1:1.9-2.1;
the preparation process of the antibacterial ceramic material comprises the following steps:
step 1), weighing the raw materials in proportion, and adding water to mix to obtain mixed slurry;
step 2), rotary steaming and concentrating the mixed slurry to obtain mud cakes;
step 3), drying the mud cake to obtain a blank;
and 4) placing the blank into a mould for compaction, heating to 900-1000 ℃, keeping the temperature for 15-30min, heating to 1300-1350 ℃, keeping the temperature for 60-90min, heating to 1450-1500 ℃, keeping the temperature for 60-90min, cooling to room temperature at a speed of 1.2-1.4 ℃/min, and demoulding to obtain the antibacterial ceramic material.
2. An antimicrobial ceramic material according to claim 1, wherein: the mass ratio of the alumina, the clay, the stabilizer, the fluxing agent, the bacteriostat and the toughening agent is 94:3:0.5:1:0.5:1.
3. an antimicrobial ceramic material according to claim 1, wherein: the stabilizer is a compound of gadolinium oxide, yttrium oxide and lanthanum oxide.
4. An antimicrobial ceramic material according to claim 3, wherein: the mass ratio of gadolinium oxide to yttrium oxide to lanthanum oxide is 0.9-1.1:2.9-3.1:1.9-2.1.
5. An antimicrobial ceramic material according to claim 1, wherein: the fluxing agent is a compound of zirconium oxide and titanium oxide.
6. An antimicrobial ceramic material according to claim 5, wherein: the mass ratio of the zirconia to the titania is 2.9-3.1:1.9-2.1.
7. An antimicrobial ceramic material according to claim 1, wherein: the bacteriostatic agent is a compound of zinc oxide and silver ion bacteriostatic agent.
8. An antimicrobial ceramic material according to claim 7, wherein: the mass ratio of the zinc oxide to the silver ion bacteriostat is 0.9-1.1:1.9-2.1.
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| KR20160102799A (en) * | 2015-02-23 | 2016-08-31 | 김영준 | Alumina ceramics composition having low sintering temperature and manufacturing process thereof |
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| CN113860857A (en) * | 2021-09-10 | 2021-12-31 | 湖北泉端新材料科技有限公司 | Alumina ceramic composite material and preparation method and application thereof |
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| KR20160102799A (en) * | 2015-02-23 | 2016-08-31 | 김영준 | Alumina ceramics composition having low sintering temperature and manufacturing process thereof |
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