CN110449332A - A kind of composite construction diamond thin and preparation method thereof - Google Patents
A kind of composite construction diamond thin and preparation method thereof Download PDFInfo
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- CN110449332A CN110449332A CN201910742679.4A CN201910742679A CN110449332A CN 110449332 A CN110449332 A CN 110449332A CN 201910742679 A CN201910742679 A CN 201910742679A CN 110449332 A CN110449332 A CN 110449332A
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- diamond
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/002—Processes for applying liquids or other fluent materials the substrate being rotated
- B05D1/005—Spin coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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Abstract
The invention discloses a kind of composite construction diamond thins and preparation method thereof, composite construction diamond thin is adhered in substrate by diamond particles and is constituted, the composite construction diamond thin includes silica solution, solvent and surface-functionalized bortz powder, it is formed by solgel reaction using diamond particles as core, silica solution is the film of network carrier, preparation method includes the following steps, surface-functionalized diamond particles powder is provided, silica sol precursor, solvent, deionized water, acid catalyst, base catalyst and destination carrier, the diamond particles powder is made annealing treatment, diamond particles powder after annealing is added solvent and is ultrasonically treated, form the diamond particles solution of stable dispersion.The present invention prepares film using the method for collosol and gel, and film wearability is good, and antibiotic property is good, and performance is stablized, and preparation method and simple process prepare diamond thin compared to PVD and CVD, and cost of the invention is low, is suitble to large-scale production.
Description
Technical field
The present invention relates to thin diamond technical field of membrane more particularly to a kind of composite construction diamond thin and its preparation sides
Method.
Background technique
Membrane electrode and antibacterial film play always important role in our daily life.Currently, in physics, changing
It learns, material and medicine and other fields have obtained relatively broad application.
Diamond thin has a wide range of applications by feat of the characteristics such as wearability and high heat conductance in film and film applications
Prospect.In addition to this, diamond possesses negative electron affinity (NEA) and surface-functionalized potentiality.The diamond table of negative electron affinity (NEA)
Releasably a large amount of electronics can generate a degree of inhibiting effect to electrically charged bacterium in face；The diamond surface of annealing can
Active oxygen-containing group is generated, these groups can promote the interaction of diamond and bacterial structure component, also can reach antibacterial
Effect.Therefore, diamond has good antibacterial property energy.
Secondly, mainly being prepared using the methods of CVD, PVD method in the method for preparing diamond thin.But these methods
Higher cost is not easy large-scale industrial production.It is at low cost and be easy to scale however, sol-gal process is by feat of easy to operate
The advantages such as production, become one of effective industrial technology method of field of film preparation.
Summary of the invention
In order to solve the technical problems such as existing diamond thin preparation cost height and low efficiency, the present invention uses for reference collosol and gel
Method prepares the thinking of sull and prepares diamond thin to design, a kind of composite construction diamond thin provided by the invention
And preparation method thereof, preparation method is simple, and thin film stability is good.
A kind of diamond thin proposed by the present invention, the diamond thin are adhered to structure in substrate by diamond particles
Include silica solution, solvent and surface-functionalized bortz powder at, the diamond thin, by solgel reaction formed with
Diamond particles are core, and silica solution is the film of network carrier.
A kind of composite construction diamond thin proposed by the present invention and preparation method thereof, comprising the following steps:
S1: diamond particles powder, silica sol precursor, solvent, deionized water, acid catalyst, base catalyst and target are provided
Carrier；
S2: the diamond particles powder is made annealing treatment, and the diamond particles powder after annealing is added solvent and is surpassed
Sonication forms the diamond particles solution of stable dispersion；
S3: the silica sol precursor, solvent, deionized water and acid catalyst are mixed, carry out that reaction is stirred at room temperature, tentatively
Obtain silica solution；
S4: the solvent, deionized water and base catalyst are added in the silica solution, is stirred at room temperature, is obtained most
Whole silica solution；
S5: the diamond particles solution is added in the silica solution, continues to be stirred at room temperature to obtain diamond thin
Agent；
S6: the membrane agent is spun in the destination carrier, by being freeze-dried and making annealing treatment, obtains the gold
Hard rock film.
Further, the silica sol precursor is selected from including methyl orthosilicate, ethyl orthosilicate, tetraethyl orthosilicate, just
Silicic acid propyl ester, methyltriethoxysilane or isocyanatopropyl triethoxysilane it is any one or more.
Further, the solvent is selected from including ethyl alcohol, one kind of isopropanol or n-butanol or three kinds, according to molar ratio 3:
The ratio of 4:1 mixes.
Further, the acid catalyst is selected from any one or more, the institute including hydrochloric acid, nitric acid, oxalic acid or citric acid
It states base catalyst and is selected from ammonium hydroxide, it includes that glass, metal, ceramics and plastics etc. are any one or more that the destination carrier, which is selected from,.
Further, during making annealing treatment in the S2, temperature is 50 to 900 DEG C, and the time is 3~6h.Described
During ultrasonic treatment, ultrasonic time 30min, the concentration of the diamond solution is 1~3g/L.
Further, silica sol precursor in the S3, solvent, deionized water molar ratio be 1:3.5~4:1, the acid
Catalyst adjusts solution ph to 2~4, and the time being stirred at room temperature is 1~2.5h.
Further, the solvent and water added in the S4 make silica sol precursor, solvent, final mole of deionized water
Proportion is 1:8~9:4, and the base catalyst adjusts solution ph to 7 or so, and the time being stirred at room temperature is 1~2h.
Further, the mass fraction that diamond solution is added in the S5 is 5%~10%, and being stirred at room temperature the time is
1h。
Further, spin coating is carried out using spin coater in the S6, speed parameter is 1500r/min, and spin-coating time is
30s, the time of the freeze-drying are that for 24 hours, the temperature of the annealing is 350~400 DEG C, and the time of annealing is 1h.
The invention has the benefit that
1, the present invention prepares film using the method for collosol and gel, and film wearability is good, and antibiotic property is good, and performance is stablized, system
Preparation Method and simple process；
2, the present invention prepares film using the method for collosol and gel, prepares diamond thin, this hair compared to PVD and CVD
Bright cost is low, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is a kind of preparation flow structural representation of composite construction diamond thin proposed by the present invention and preparation method thereof
Figure.
In figure: tank shell on 1,2 water pipes, 3 shafts, 4 curved bars, 5 injection molded tubes, 6 top covers, 7 suction heads, 8 air-breathing casings,
9 fixed blocks, 10 springs, 11 sliding blocks, 12 connecting holes.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig.1, a kind of composite construction diamond thin and preparation method thereof, comprising the following steps:
S1: diamond particle surfaces layer carries out corona treatment, adulterates N, S element in superficial layer, realizes negative electron parent
With energy surface structure function.
S2: surface-functionalized diamond particles powder, silica sol precursor, solvent, deionized water, acid catalyst, alkali are provided
Catalyst and destination carrier.It includes methyl orthosilicate, ethyl orthosilicate, positive silicic acid tetrem that wherein the silica sol precursor, which is selected from,
Ester, positive silicic acid propyl ester, methyltriethoxysilane or isocyanatopropyl triethoxysilane it is any one or more, the acid is urged
Agent is selected from including any one or more of hydrochloric acid, nitric acid, oxalic acid or citric acid, and it includes glass, gold that the destination carrier, which is selected from,
Category, ceramics and plastics etc. are any one or more；
S2: it by the surface-functionalized diamond particles powder in 50 to 900 DEG C of at a temperature of 3~6h of annealing, moves back
Bortz powder after fire is added solvent supersonic and handles 30min, forms the diamond solution for the stable dispersion that concentration is 1~3g/L；
S3: the silica sol precursor, solvent, deionized water are mixed with the molar ratio of 1:3.5~4:1, the acid catalysis
Agent adjusts solution ph to 2~4, and the time being stirred at room temperature is 1~2.5h, tentatively obtains silica solution；
S4: adding the solvent, deionized water and base catalyst in the silica solution colloidal sol, makes silica sol precursor, molten
Agent, deionized water final mol ratio be 1:8~9:4, the base catalyst adjusts solution ph to 7 or so, is stirred at room temperature 1
~2h obtains final silica solution；
S5: the diamond solution of 5%~10% (mass fraction) is added in the silica solution, continues to be stirred at room temperature
1h obtains thin diamond film；
S6: the membrane agent is spun in the destination carrier with the speed parameter of 1500r/min on spin coater, rotation
The painting time is 30s, is annealed in air 1h after freeze-drying for 24 hours with 350~400 DEG C of temperature, to obtain the diamond
Film.
Embodiment 1:
The surface-functionalized diamond particles powder of 0.03g is put into crucible, is annealed in air with 450 DEG C of temperature
3h.Diamond particles powder is dispersed in 10ml isopropanol again, is ultrasonically treated 30min；
10.416g ethyl orthosilicate, 11.712g isopropanol and 0.9g deionized water are uniformly mixed, hydrochloric acid is added dropwise and adjusts
1.5h is stirred at room temperature to 2~4 in pH value.15.315g isopropanol and 2.7g deionized water are added in above-mentioned solution, ammonia is added dropwise
Water adjusts pH to neutrality, and 1.5h is stirred at room temperature and obtains silica solution；
The diamond solution handled well is uniformly mixed with the silica solution, 1h is stirred at room temperature, obtains target thin film.It will
The membrane agent is spun in the destination carrier with the speed parameter of 1500r/min on spin coater, spin-coating time 30s, cold
Be lyophilized it is dry for 24 hours after annealed in air 1h with 350~400 DEG C of temperature, to obtain composite construction diamond thin.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of composite construction diamond thin, which is characterized in that the composite construction diamond thin is glued by diamond particles
It is attached in substrate and constitutes, the composite construction diamond thin includes silica solution, solvent and surface-functionalized bortz powder, warp
It crosses solgel reaction to be formed using surface-functionalized diamond particles as core, silica solution is the film of network carrier.
2. a kind of preparation method of composite construction diamond thin, which comprises the following steps:
S1: surface-functionalized diamond particles powder, silica sol precursor, solvent, deionized water, acid catalyst, base catalysis are provided
Agent and destination carrier；
S2: carrying out superficial layer plasma doping N, S element for the diamond particles powder, realizes the affine energy surface knot of negative electron
Structure functionalization.
S3: and then surface-functionalized diamond particles powder is made annealing treatment, the surface-functionalized diamond after annealing
Grain powder is added solvent and is ultrasonically treated, and forms the diamond particles solution of stable dispersion；
S4: the silica sol precursor, solvent, deionized water and acid catalyst are mixed, carries out that reaction is stirred at room temperature, tentatively obtains
Silica solution；
S5: adding the solvent, deionized water and base catalyst in the silica solution, be stirred at room temperature, and obtains final
Silica solution；
S6: the surface-functionalized diamond particles solution is added in the silica solution, continues to be stirred at room temperature to obtain gold
Hard rock membrane agent；
S7: the membrane agent is spun in the destination carrier, by being freeze-dried and making annealing treatment, obtains the composite junction
Structure diamond thin.
3. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that in the S1
Silica sol precursor be methyl orthosilicate, ethyl orthosilicate, tetraethyl orthosilicate, positive silicic acid propyl ester, methyltriethoxysilane or
Isocyanatopropyl triethoxysilane any contains any one of them.
4. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that in the S1
Prepared silica solution mass percentage content is that 10%~65%, SiO2 nano particle diameter is 5nm~50nm.
5. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that diamond
Grain superficial layer plasma doping N, S element realizes the affine energy surface structure function of negative electron.
6. a kind of preparation method of composite construction diamond coatings film according to claim 2, which is characterized in that described
It is 50 DEG C~900 DEG C that diamond particle surfaces, which carry out annealing annealing temperature in air, in S2, and annealing time is 3~6h.
7. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that the preparation
Silica solution in prepare silica solution mass percentage be 30~65%.
8. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that the solvent
For one kind of ethyl alcohol, isopropanol or n-butanol or three kinds, mixed according to the ratio of molar ratio 3:4:1.
9. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that the Buddha's warrior attendant
The mass fraction that the stable dispersions of stone particle are added in silica solution is 5%~10%, and the diameter range of diamond particles is 5
Nanometer~100 microns.
10. a kind of preparation method of composite construction diamond thin according to claim 2, which is characterized in that the gold
There are antibacterial functions after the processing of hard rock film surface annealing process.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029317A (en) * | 2020-09-03 | 2020-12-04 | 上海金铎禹辰水环境工程有限公司 | Preparation method of diamond particle coating paint |
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