CN208346252U - Metal mesh deposition of diamond coatings device and metal mesh deposition of diamond coatings system - Google Patents
Metal mesh deposition of diamond coatings device and metal mesh deposition of diamond coatings system Download PDFInfo
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- CN208346252U CN208346252U CN201820338175.7U CN201820338175U CN208346252U CN 208346252 U CN208346252 U CN 208346252U CN 201820338175 U CN201820338175 U CN 201820338175U CN 208346252 U CN208346252 U CN 208346252U
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Abstract
本实用新型公开了一种金属网沉积金刚石涂层装置和金属网沉积金刚石涂层系统，涉及油水分离金刚石涂层金属网技术领域。金属网沉积金刚石涂层装置包括夹具本体；夹具本体包括平行设置的第一本体和第二本体，第一本体和第二本体的本体内部均独立地具有空洞，金属网置于第一本体与第二本体之间，且金属网边缘尺寸大于第一本体和第二本体的空洞尺寸，第一本体与第二本体通过垂直于第一本体的可拆卸夹紧机构固定，以夹紧金属网。本实用新型缓解了化学气相沉积沉积温度较高，由于金属网较薄，在沉积过程中容易变形，造成沉积和薄膜生长不均匀的缺陷，通过本实用新型可以将金属网固定住，沉积过程金属网不会变形，使金属网上生长的金刚石薄膜更加均匀。
The utility model discloses a metal mesh deposition diamond coating device and a metal mesh deposition diamond coating system, which relate to the technical field of oil-water separation diamond coating metal mesh. The metal mesh deposition diamond coating device includes a fixture body; the fixture body includes a first body and a second body arranged in parallel, the inside of the first body and the second body are independently hollow, and the metal mesh is placed on the first body and the second body. Between the two bodies, and the size of the edge of the metal mesh is larger than the size of the cavity of the first body and the second body, the first body and the second body are fixed by a detachable clamping mechanism perpendicular to the first body to clamp the metal mesh. The utility model alleviates the high deposition temperature of chemical vapor deposition. Because the metal mesh is thin, it is easy to deform during the deposition process, resulting in uneven deposition and film growth defects. The metal mesh can be fixed by the utility model. The mesh will not deform, making the diamond film grown on the metal mesh more uniform.
Description
Technical field
The utility model relates to water-oil separating diamond coatings metal mesh technical fields, in particular to a kind of metal
Net deposition of diamond coatings device and metal mesh deposition of diamond coatings system.
Background technique
Since the new century, oily water separation technique is obtained in multiple fields such as petrochemical industry, sewage treatment, food engineerings
To extensive use.Current oily waste water mainly uses the methods of gravitational settling, coarse, centrifuge separation to carry out two stage treatment,
Although these methods are capable of handling oily waste water, but have the shortcomings that low separation efficiency, at high cost, the rate of recovery is low etc..Water-oil separating
It is the essential industry process for administering oily waste water and aqueous oil liquid.Water-oil separating is completely different to oil and water using same material
Wellability and be separated from water oil, such as material has super-hydrophobic super-oleophylic property or with superhydrophilic superoleophobic
Matter.The exploitation research and development of subsequent super-hydrophobicity and super-oleophilic filtering material are gradually goed deep into, these filtering material oleophilic drainages.Generally
Method be the porous structure of decorative material be it is super-hydrophobic, and in various porous structures, wire mesh is due to its low cost, high machine
Tool intensity and porous structure become ideal material.
Common metal net can be modified in such a way that surface is modified on the surface of metallic netted structural, and acid can be used
The method of caustic corrosion is modified processing using surface modifier, and it is super-hydrophobic to change surface texture induction typically by corrosion
Super-oleophilic matter, such as metal copper mesh is corroded in nitric acid solution, increase the roughness on copper wire surface, and pass through modification 16
Alkanethiol makes it have super-hydrophobic super-oleophylic property, and this method can obtain the effect of water-oil separating.
And the organism kinds as contained in oil mixing with water state, grease content, oil-water mixture, water-oil separating object
The difference of equal many factors, causes water-oil separating difficulty to become increasing.The surface modification of metal mesh progress simultaneously makes it have
The characteristic of hydrophobic oleophilic oil also encounters many restrictions in practical applications: firstly, metal mesh corrosion resistant performance itself is limited, being easy quilt
Environment is corroded, and service life is shorter；Secondly, metal net surface is modified stronger applied to specificity in water-oil separating, for
Oil type it is less, specific water-oil separating needs corresponding specific corrosion and modifier treatment；Again, pass through acid and alkali corrosion
Or when using the method progress water-oil separating of surface modifying agent, the time cannot very persistently, acid and alkali corrosion and addition surface
The hydrophobic functional group that the method for modifying agent is added in metal surface only on surface, is easy failure.
Diamond is substance most hard in the world, possesses extremely stable physicochemical properties and higher elasticity modulus.
Deposition of diamond coatings can make metal mesh obtain hydrophobicity and/or hydrophily on metal mesh, since diamond is with high
Physical and chemical stability, not only can be with the corrosion of strong alkali-acid resistance etc., but also the high rigidity of diamond and elasticity modulus all may be used
To greatly improve its service life.Patent CN103741116A proposes one kind and grows cvd diamond painting on metal mesh substrate
Layer makes diamond mesh surface have super-hydrophobicity and hydrophilic method, but this method process is complicated, and used deposition is set
It is standby expensive, at high cost, can only on small size workpiece long diamond thin, be unfavorable for industrialized production and industrial use.
Chemical vapor deposition (Chemical Vapor Deposition, CVD) mode depositing diamond is mainly used at present
Coating, but temperature is higher when deposition, since metal mesh is relatively thin, is easily deformed during the deposition process, causes deposition uneven, it is thin
Film growth is uneven, reduces the oil-water separation of diamond coatings metal mesh.
In view of this, special propose the utility model.
Utility model content
One of the purpose of this utility model is to provide a kind of metal mesh deposition of diamond coatings device, apparatus structure letter
It is single, metal mesh can be fixed by using the device, deposition process metal mesh will not deform, and be highly suitable for three-dimensional
On chemical vapor deposited coatings preparation.
The two of the purpose of this utility model are to provide a kind of comprising the metal mesh deposition of diamond coatings device
Metal mesh deposition of diamond coatings system has advantage identical with above-mentioned metal mesh deposition of diamond coatings device.
In order to realize the above-mentioned purpose of the utility model, the following technical scheme is adopted:
In a first aspect, a kind of metal mesh deposition of diamond coatings device is provided, the metal mesh deposition of diamond coatings
Device includes chuck body；
The chuck body includes the first noumenon disposed in parallel and the second ontology, the first noumenon and second described
The body interior of body independently has cavity, and metal mesh is placed between the first noumenon and second ontology, and metal
Network edge size is greater than the pore size of the first noumenon and second ontology, the first noumenon and second ontology
Fixed by the detachable clamp system perpendicular to the first noumenon, with clamp the first noumenon and second ontology it
Between metal mesh.
Preferably, on the basis of technical solutions of the utility model, the first noumenon and second ontology are molybdenum
Disk.
Preferably, on the basis of technical solutions of the utility model, the detachable clamp system includes screw bolt and nut.
Preferably, on the basis of technical solutions of the utility model, the chuck body further includes the first spring leaf or
Two spring leafs (142)；
First spring leaf is located on the inside of the first noumenon；
Second spring piece is located on the inside of second ontology.
Preferably, on the basis of technical solutions of the utility model, the chuck body further includes the first spring leaf and
Two spring leafs；
First spring leaf is located on the inside of the first noumenon；
The second spring piece is located on the inside of second ontology.
Second aspect provides a kind of metal mesh deposition Buddha's warrior attendant comprising the metal mesh deposition of diamond coatings device
Stone coat system.
Preferably, on the basis of technical solutions of the utility model, the metal mesh deposition of diamond coatings system includes
Vacuum system and the reaction chamber being connected with the vacuum system；
Hot wire heater is equipped in the reaction chamber；The hot wire heater includes upper and lower heat extraction silk；The metal mesh is heavy
Product diamond coatings device is as between upper and lower heat extraction silk.
Preferably, on the basis of technical solutions of the utility model, gas distributor is equipped with above the hot wire heater；
The gas distributor includes hydrogen chamber, methane gas chamber and water cooling chamber；The hydrogen chamber is equipped with hydrogen paths, is used for
It is passed through hydrogen；The methane gas chamber is equipped with methane channel, for being passed through methane gas；The water cooling chamber is equipped with water inlet and water outlet
Mouthful, for being passed through cooling water.
Preferably, on the basis of technical solutions of the utility model, the heated filament of the hot wire heater (300) is tungsten wire；
The tungsten wire diameter is 1-3mm.
Preferably, on the basis of technical solutions of the utility model, the vertical range between the heat extraction silk up and down is 30-
40mm；
Wherein, vertical range of the upper heat extraction flight lead from metal mesh is 20-25mm.
Compared with the prior art, the utility model has the following beneficial effects:
The apparatus structure for being suitble to deposit nano diamond coating in metal mesh surface three dimension of the utility model design is simple,
Metal mesh can be fixed, effectively prevent metal mesh in deposition process to deform, the chemical gas being highly suitable on three-dimensional
The preparation of phase depositing coating.Meanwhile it can make to deposit by using the metal mesh deposition of diamond coatings device of the utility model
The depositing temperature of metal mesh in the process is more uniform, so that it is more uniform to obtain diamond film growth, obtained diamond
The oil-water separation of coating metal net is good, and separative efficiency is high.
Detailed description of the invention
Fig. 1 is a kind of top view of the metal mesh deposition of diamond coatings device of embodiment of the utility model；
Fig. 2 is a kind of main view of the metal mesh deposition of diamond coatings device of embodiment of the utility model；
Fig. 3 is 1 metal mesh surface topography map of the utility model embodiment；
Fig. 4 is the diamond film surface shape appearance figure grown on 1 metal mesh of the utility model embodiment.
Icon: 100- chuck body；110- the first noumenon；The second ontology of 120-；The detachable clamp system of 130-；131- spiral shell
Bolt；132- nut；The first spring leaf of 141-；142- second spring piece；200- metal mesh；300- hot wire heater.
Specific embodiment
The technical solution of the utility model is clearly and completely described below in conjunction with attached drawing, it is clear that described
Embodiment is the utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those of ordinary skill every other embodiment obtained without making creative work belongs to practical
Novel protected range.
First aspect according to the present utility model, provides a kind of metal mesh deposition of diamond coatings device, and Fig. 1 is this
A kind of top view of the metal mesh deposition of diamond coatings device of embodiment of utility model；Fig. 2 is a kind of reality of the utility model
Apply the main view of the metal mesh deposition of diamond coatings device of mode.As depicted in figs. 1 and 2, metal mesh deposition of diamond coatings
Device includes chuck body 100；Chuck body 100 includes the first noumenon 110 disposed in parallel and the second ontology 120, first
The body interior of body 110 and the second ontology 120 independently has cavity, and metal mesh 200 is placed in the first noumenon 110 and second
Between body 120, and 200 marginal dimension of metal mesh is greater than the pore size of the first noumenon 110 and the second ontology 120；The first noumenon
110 and second ontology 120 it is fixed by the detachable clamp system 130 perpendicular to the first noumenon 110, to clamp the first noumenon
110 and the second metal mesh 200 between ontology 120.
Metal mesh 200 is placed between the first noumenon 110 and the second ontology 120 when use, with detachable clamp system 130
The first noumenon 110 and the second ontology 120 are clamped, thus the metal mesh 200 between clamping, due to the first noumenon 110 and second
It is empty, pore size of 200 marginal dimension of metal mesh greater than the first noumenon 110 and the second ontology 120, gold among ontology 120
Belonging to net 200 can be by frame between the first noumenon 110 and the second ontology 120.Empty shape is unlimited, as long as 200 edge of metal mesh
It will not be scurried out between the first noumenon 110 and the second ontology 120 by frame, form a fixture.When depositing coating, this is filled
It is placed in substrate position.
The method of typical but non-limiting depositing coating is chemical vapor deposition (Chemical Vapor
Deposition, CVD) method, including HF CVD, microwave plasma CVD or flame combustion process etc..
Typical but non-limiting metal mesh is, for example, copper mesh, titanium net or stainless (steel) wire.
It is applied when carrying out Diamond coating deposition on metal mesh by using the metal mesh depositing diamond of the utility model
Layer device can fix metal mesh, effectively prevent metal mesh in deposition process to deform, while making the metal in deposition process
The depositing temperature of net is more uniform, so that it is more uniform to obtain diamond film growth.Since metal net surface Direct precipitation goes out
Nano diamond coating with hydrophobic oleophilic oil makes metal mesh have super good hydrophobic oleophilic oil property, obtained diamond coatings
The oil-water separation of metal mesh is good, and separative efficiency is high.
The apparatus structure for being suitble to deposit nano diamond coating in metal mesh surface three dimension of the utility model design is simple,
Preparation suitable for the chemical vapor deposited coatings on three-dimensional.It is not only suitable for the deposition in small size workpiece, also suitable pair
Large-area metal net carries out batch deposition, is suitble to industrialized production and industrial applications.
In a preferred embodiment, the first noumenon and the second ontology are molybdenum disk.
Molybdenum fusing point is high, can keep high-intensitive under high temperature, while having high elastic modulus and low weight, be chuck body
Ideal carrier material.
In a preferred embodiment, detachable clamp system 130 includes bolt 131 and nut 132.
Detachable clamp system includes more set screw bolt and nut, and multiple bolts pass through parallel the first noumenon and second
Body, and with the distance between nut adjustment the first noumenon and the second ontology, it is tightened, intermediate metal mesh is clamped, by metal
Net is fixed, to prevent from deforming under metal mesh high temperature, makes to deposit more uniform.
In a preferred embodiment, chuck body 100 further includes the first spring leaf 141 or second spring piece 142；
First spring leaf 141 is located at 110 inside of the first noumenon；Second spring piece 142 is located at 120 inside of the second ontology.
In a preferred embodiment, chuck body 100 further includes the first spring leaf 141 and second spring piece 142；
First spring leaf 141 is located at 110 inside of the first noumenon；Second spring piece 142 is located at 120 inside of the second ontology.
Here inside refers to the side of metal mesh and body contacts.
By the first spring leaf of setting and/or second spring piece, appearance when metal mesh is fixed with bolt and nut can be avoided
Gap makes metal mesh be fixedly clamped stronger, metal mesh is further prevented to deform.
The second aspect according to the present utility model provides a kind of comprising the metal mesh deposition of diamond coatings dress
The metal mesh deposition of diamond coatings system set.
Metal mesh deposition of diamond coatings system has advantage identical with above-mentioned metal mesh deposition of diamond coatings device,
This is repeated no more again.
In a preferred embodiment, metal mesh deposition of diamond coatings system include vacuum system and with vacuum system
The reaction chamber that system is connected；Hot wire heater 300 is equipped in reaction chamber；Hot wire heater includes upper and lower heat extraction silk；Metal mesh is heavy
Product diamond coatings device is as between upper and lower heat extraction silk.
Using heated filament vapor deposition mode deposition of diamond coatings on metal mesh.Hot filament CVD temperature is logical
Normal more other methods (such as microwave method, flame combustion process) are low, are a kind of methods of low-temperature epitaxy Nano diamond, can be effective
Avoid the deformation of metal mesh during the deposition process.It is compared with other methods, this method rate of film build is fast, depositing device is simple, suitable
Close extensive deposition, preparation process is simple, process stabilizing, at low cost, and industrialized production and heavy industrialization is suitble to use.It adopts
With the effect of hot-wire chemical gas-phase deposition, three-dimensional (all directions) grow diamond coatings on metal mesh, and this method is prepared into
The diamond coatings metal mesh hydrophobic oleophilic oil arrived, can be applied in water-oil separating, water-oil separating is high-efficient；Since diamond has
High physical and chemical stability, not only can be with the corrosion of strong alkali-acid resistance etc., but also the high rigidity and elasticity modulus of diamond
The service life of metal mesh itself can be greatly improved.
In a preferred embodiment, gas distributor is equipped with above hot wire heater 300；Gas distributor includes
Hydrogen chamber, methane gas chamber and water cooling chamber；Hydrogen chamber is equipped with hydrogen paths, for being passed through hydrogen；Methane gas chamber is equipped with methane channel,
For being passed through methane gas；Water cooling chamber is equipped with inlet and outlet, for being passed through cooling water.
It needs to be passed through CH in deposition process4And H2, wherein CH4Carbon source, H are provided for the growth of diamond2Generate active hydrogen-based
Group-H removes the SP of etching non-diamond phase2Key.
Preferably, control hydrogen paths pelvic outlet plane is to the upper heat extraction silk plan range of hot wire heater in 3-5mm.
By the distance between the outflow of control hydrogen and heated filament, H can be made2Active hydrogen group-H is generated preferably to go to etch
The SP of non-diamond phase2Key obtains the diamond thin of better quality.
In a preferred embodiment, the heated filament of hot wire heater 300 is tungsten wire；Tungsten wire diameter is 1-3mm, such as
1mm, 2mm or 3mm.
Tungsten wire fusing point is high, and resistivity and temperature-coefficient of electrical resistance degree are also higher, can be added with less energy by tungsten wire is cracking
Heat arrives depositing temperature, saves energy.
In a preferred embodiment, the vertical range between upper and lower heat extraction silk be 30-40mm, such as 30mm,
32mm, 34mm, 35mm, 36mm, 38mm or 40mm；
Wherein, vertical range of the upper heat extraction flight lead from metal mesh 200 be 20-25mm, for example, 20mm, 21mm, 22mm,
23mm, 24mm or 25mm.
By controlling the depositing temperature for guaranteeing metal mesh with a distance from sample of upper and lower heat extraction silk, keep depositing temperature preferably more
Uniformly.
Preferably, a kind of preparation method of diamond coatings metal mesh, comprising the following steps:
Using above-mentioned metal mesh deposition of diamond coatings system by hot-wire chemical gas-phase deposition mode in metal netlist
Face deposition of diamond coatings.
Preferably, reaction chamber temperature is 500-800 DEG C, for example, 500 DEG C, 550 DEG C, 600 DEG C, 650 DEG C, 700 DEG C, 750
DEG C or 800 DEG C.
Preferably, reaction chamber temperature rises to 500-800 DEG C from room temperature with the heating rate of 15-25 DEG C/min, and keeps the temperature 10-
20min。
Typical but non-limiting heating rate is, for example, 15 DEG C/min, 20 DEG C/min or 25 DEG C/min.
Typical but non-limiting soaking time is, for example, 10min, 15min or 20min.
Reaction chamber temperature is lower when hot-wire chemical gas-phase deposition, further alleviates metal mesh and is easy to become during the deposition process
Shape leads to the defect that cannot effectively deposit.
Preferably, gas distributor further includes inert gas；Typical but non-limiting inert gas is argon gas.
The total flow that hydrogen, methane gas and inert gas are controlled in reaction process is 400-600mL/min, wherein methane
Gas flow accounts for the 1-5% of total flow, and hydrogen flowing quantity accounts for the 25-45% of total flow, and inert gas flow accounts for the 50- of total flow
70%.
It is high-quality, attached to grow by control total flow and the flow accounting of hydrogen, methane gas and inert gas
Put forth effort strong nano-diamond film.Hydrogen is very few to be unfavorable for generating the SP that active hydrogen group-H goes etching non-diamond phase2Key,
CH4Gas is very few cannot to provide sufficient carbon source for the growth of diamond.
Preferably, deposition pressure is 1500-2000Pa when deposition.
By controlling deposition pressure, it help to obtain the film layer of high quality, the diamond thin compact structure of growth.
Preferably, sedimentation time control is in 1.5-3h, for example, 1.5h, 2h, 2.5h or 3h.
It is suitable for that adhesive force is preferable by controlling the thin diamond film thickness that sedimentation time is grown.
In a preferred embodiment, using hot-wire chemical gas-phase deposition mode in metal net surface depositing diamond
Nano diamond is carried out to metal mesh before coating and plants brilliant processing.
Planting brilliant processing is to be previously implanted one layer of small diamond particles as nucleating point, to improve Buddha's warrior attendant in matrix surface
Stone settled density.
The brilliant processing mode of typical but non-limiting plant is to be surpassed with the suspension containing diadust to substrate surface
Sonication.
Preferably, it plants brilliant processing and takes out drying for metal mesh to be put into the brilliant solution of plant after ultrasound 20-60min, it is preferably dry
It is dry for being dried with nitrogen.
Typical but non-limiting ultrasonic time is, for example, 20min, 30min, 40min, 50min or 60min.
Preferably, planting brilliant solution is nanodiamond suspension；It is preferred that nanodiamond suspension includes Nano diamond
Powder, dimethyl carbonate and water, nano-diamond powder quality account for the 0.005-0.01% of nanodiamond suspension quality, carbonic acid two
Concentration of the methyl esters in nanodiamond suspension is 1 × 10-6-10×10-6mol/L；It is preferred that the pH of nanodiamond suspension
For 2-4.
Nanodiamond suspension is that nano-diamond powder is scattered in the solvent of dimethyl carbonate and water, Nano diamond
Powder mass fraction is 0.005-0.01%, such as 0.005%, 0.006%, 0.007%, 0.008%, 0.009% or 0.01%.
Dimethyl carbonate (DMC) concentration is 1 × 10-6mol/L、2×10-6mol/L、3×10-6mol/L、4×10-6mol/L、5×10- 6mol/L、6×10-6mol/L、7×10-6mol/L、8×10-6mol/L、9×10-6Mol/L or 10 × 10-6mol/L.Nanogold
The pH of hard rock suspension is 2-4, such as pH2, pH3 or pH4.
Metal mesh is carried out to remain in metal after planting brilliant processing by using the nanodiamond suspension (planting brilliant solution)
The clast of diadust in netlist planar defect can provide nucleation core for hot filament CVD depositing diamond,
Enhancing Nucleation Density is improved, the adhesive force of diamond thin and substrate is significantly improved.
In a preferred embodiment, the preparation method of diamond coatings metal mesh, comprising the following steps:
(a) metal net surface is cleaned；
(b) corrosion treatment is carried out to cleaned metal mesh；
(c) metal mesh is cleaned again；
(d) Nano diamond is carried out to metal mesh and plants brilliant processing；
(e) above-mentioned metal mesh deposition of diamond coatings system is used to pass through hot-wire chemical gas-phase deposition side after planting brilliant processing
Formula obtains diamond coatings metal mesh in metal net surface deposition of diamond coatings；
Preferably, step (a) includes first being cleaned by ultrasonic 2-3 times, each 5-10min with water, then be cleaned by ultrasonic 1-2 with alcohol
It is secondary, each 5-10min.
First metal net surface is cleaned, removes the impurity of metal net surface, keeps specimen surface clean.
Preferably, step (b) includes the first ultrasound 5-10min in aqueous slkali, then the ultrasound 30-60s in acid solution；It is excellent
Selecting aqueous slkali is the NaOH solution of 0.5-1mol/L；It is preferred that acid solution is the HCl solution of 0.5-1mol/L.
The first ultrasound 5-10min in aqueous slkali, such as 5min, 6min, 7min, 8min, 9min or 10min, then in acid
Ultrasound 30-60s in solution, such as 30s, 40s, 50s or 60s.
Alkaline concentration is, for example, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or 1mol/L；
Acid solutions are, for example, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or 1mol/L.
Corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, improves the adsorption density of diamond particles.
Preferably, step (c) includes first being cleaned by ultrasonic 2-3 times, each 5-10min with water, then be cleaned by ultrasonic 1-2 with alcohol
It is secondary, each 5-10min.
Metal mesh after corrosion treatment is cleaned, the etchant solution remained in metal mesh is cleaned up.
Preferably, step (d) includes being put into metal mesh in the brilliant solution of plant to take out drying after ultrasound 20-60min, preferably dry
It is dry for being dried with nitrogen；It is preferred that planting brilliant solution is nanodiamond suspension；Preferably include nano-diamond powder, dimethyl carbonate
And water, nano-diamond powder quality account for the 0.005-0.01% of nanodiamond suspension quality, dimethyl carbonate is in nanogold
Concentration in hard rock suspension is 1 × 10-6-10×10-6mol/L；It is preferred that the pH of nanodiamond suspension is 2-4.
The plant crystalline substance processing of diamond is carried out to metal mesh.Typical crystalline substance solution of planting is detonation nanodiamond suspension, at
It is divided into bortz powder mass fraction 0.005%, DMC concentration is 5 × 10-6M, remaining is deionized water, pH 3.Planting crystal type is
Sample is put into the brilliant solution of plant ultrasound 30 minutes, is taken out, with being dried with nitrogen.
Step (e) is using above-mentioned metal mesh deposition of diamond coatings system by hot-wire chemical gas-phase deposition mode in gold
Belong to net surface deposition of diamond coatings, deposition parameter is identical as above description.
This method increases the nucleation density and two of growth by the process for surface preparation of corrosion treatment and the brilliant processing of plant
Secondary nucleation rate obtains the film with nano-sized grains degree, and by using the metal mesh depositing diamond of the utility model
Coat system carries out Diamond coating deposition to metal mesh, and the diamond thin grown on metal mesh is uniform, high-quality, will
To diamond coatings metal mesh for separative efficiency in water-oil separating high, long service life.
Preferably, can be used for comprising oily wastewaters such as common organic solvents, vegetable and animals oils, petroleum, vapour, diesel oil and crude oil
Separation.
Preferably, diamond coatings metal mesh is placed in oil water mixture, oil can pass through diamond coatings metal mesh
And water cannot achieve the purpose that water-oil separating by diamond coatings metal mesh.
The utility model is further illustrated below by specific embodiment and comparative example, it should be understood, however, that, these
Embodiment is only for being described in more detail and be used, and but should not be understood as limiting the utility model in any form.This reality
It can be by commercially available acquisition with the novel each raw material being related to.
The metal mesh of embodiment and comparative example is copper mesh.
The detonation nanodiamond suspension ingredient that embodiment and comparative example uses is bortz powder mass fraction
0.005%, DMC concentration are 5 × 10-6M, remaining is deionized water, pH 3.
The metal mesh deposition of diamond coatings system that embodiment uses includes metal mesh deposition of diamond coatings device, vacuum
System and the reaction chamber being connected with vacuum system；Hot wire heater is equipped in reaction chamber；Hot wire heater includes upper and lower heat extraction
Silk；Heated filament is tungsten wire；Vertical range between upper and lower heat extraction silk is 30-40mm.Metal mesh deposition of diamond coatings device as
Between upper and lower heat extraction silk.Gas distributor is equipped with above hot wire heater；Gas distributor includes hydrogen chamber, methane gas chamber and argon
Gas chamber；Hydrogen chamber is for being passed through hydrogen；Methane gas chamber is for being passed through methane gas；Argon gas room is for being passed through argon gas.
Metal mesh deposition of diamond coatings device includes the chuck body between upper and lower heat extraction silk；Chuck body includes
Molybdenum disk up and down disposed in parallel has cavity among upper and lower molybdenum disk, is in square shape, it is corresponding to be equipped with shape on the inside of upper and lower molybdenum disk
Spring leaf, metal mesh are placed between the spring leaf on the inside of molybdenum disk, and metal mesh marginal dimension is greater than the pore size of upper and lower molybdenum disk, will
Bolt vertically penetrates chuck body and through upper and lower molybdenum disk, is tightened with nut, is clamped metal mesh.
Embodiment 1
A kind of preparation method of diamond coatings metal mesh, comprising the following steps:
(1) metal net surface is cleaned, is cleaned by ultrasonic 2 times using deionized water first, 5 minutes every time, is finally used
Alcohol is cleaned by ultrasonic 5 minutes, with being dried with nitrogen；
(2) corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, and improve diamond nano-particles
Adsorption density.Corrosion treatment is to be cleaned by ultrasonic in aqueous slkali 5 minutes, is then cleaned 30 seconds in acid solution.Wherein aqueous slkali
For the NaOH of 1M, acid solution is the HCl of 1M；
(3) metal mesh is cleaned, the etchant solution remained in metal mesh is cleaned up.It is super using deionized water
Sound cleans 2 times, 5 minutes every time, is finally cleaned by ultrasonic 5 minutes with alcohol, with being dried with nitrogen；
(4) the plant crystalline substance for carrying out Nano diamond to metal mesh is handled, and planting brilliant solution is detonation nanodiamond suspension, is planted
Crystal type is to be put into sample in the brilliant solution of plant ultrasound 30 minutes, is taken out, with being dried with nitrogen；
(5) three-dimensional manometer thin diamond is carried out to the metal mesh after planting crystalline substance using metal mesh deposition of diamond coatings system
The preparation of film rises to 600 DEG C from room temperature with the heating rate of 20 DEG C/min, and keeps the temperature 15min；It is total that gas is controlled in reaction process
Flow is 500mL/min, and methane+argon gas+hydrogen total flow is 500mL/min, wherein methane 10mL/min, argon gas 282mL/
Min, hydrogen 208mL/min.Pressure is 1500Pa.Upper heat extraction silk from metal mesh in metal mesh deposition of diamond coatings device away from
From 25mm, lower heat extraction silk metal mesh distance 15mm in metal mesh deposition of diamond coatings device, sedimentation time is 2 hours.
Fig. 3 is 1 metal mesh surface topography map of embodiment；Fig. 4 is the diamond film surface grown on 1 metal mesh of embodiment
Shape appearance figure.
Embodiment 2
A kind of preparation method of diamond coatings metal mesh, comprising the following steps:
(1) metal net surface is cleaned, is cleaned by ultrasonic 3 times using deionized water first, 5 minutes every time, is finally used
Alcohol is cleaned by ultrasonic 5 minutes, with being dried with nitrogen.
(2) corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, and improve diamond nano-particles
Adsorption density.Corrosion treatment is to be cleaned by ultrasonic in aqueous slkali 10 minutes, is then cleaned 60 seconds in acid solution.Wherein aqueous slkali
Are as follows: the NaOH of 0.5M, acid solution are the HCl of 0.5M.
(3) metal mesh is cleaned, the etchant solution remained in metal mesh is cleaned up.It is super using deionized water
Sound cleans 3 times, 5 minutes every time, is finally cleaned by ultrasonic 5 minutes with alcohol, with being dried with nitrogen.
(4) the plant crystalline substance for carrying out Nano diamond to metal mesh is handled, and planting brilliant solution is detonation nanodiamond suspension.It plants
Crystal type is to be put into sample in the brilliant solution of plant ultrasound 30 minutes, is taken out, with being dried with nitrogen.
(5) three-dimensional manometer thin diamond is carried out to the metal mesh after planting crystalline substance using metal mesh deposition of diamond coatings system
The preparation of film rises to 600 DEG C from room temperature with the heating rate of 20 DEG C/min, and keeps the temperature 15min；It is total that gas is controlled in reaction process
Flow is 400mL/min, and methane+argon gas+hydrogen total flow is 400mL/min, wherein methane 5mL/min, argon gas 255mL/
Min, hydrogen 140mL/min.Pressure is 1500Pa.Upper heat extraction silk from metal mesh in metal mesh deposition of diamond coatings device away from
From 25mm, lower heat extraction silk metal mesh distance 15mm in metal mesh deposition of diamond coatings device, sedimentation time is 3 hours.
Embodiment 3
A kind of preparation method of diamond coatings metal mesh, comprising the following steps:
(1) metal net surface is cleaned, is cleaned by ultrasonic 2 times using deionized water first, 10 minutes every time, is finally used
Alcohol is cleaned by ultrasonic 5 minutes, with being dried with nitrogen.
(2) corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, and improve diamond nano-particles
Adsorption density.Corrosion treatment is to be cleaned by ultrasonic in aqueous slkali 8 minutes, is then cleaned 40 seconds in acid solution.Wherein aqueous slkali
Are as follows: the NaOH of 0.6M, acid solution are the HCl of 0.6M.
(3) metal mesh is cleaned, the etchant solution remained in metal mesh is cleaned up.It is super using deionized water
Sound cleans 2 times, 10 minutes every time, is finally cleaned by ultrasonic 5 minutes with alcohol, with being dried with nitrogen.
(4) the plant crystalline substance for carrying out Nano diamond to metal mesh is handled, and planting brilliant solution is detonation nanodiamond suspension.It plants
Crystal type is to be put into sample in the brilliant solution of plant ultrasound 30 minutes, is taken out, with being dried with nitrogen.
(5) three-dimensional manometer thin diamond is carried out to the metal mesh after planting crystalline substance using metal mesh deposition of diamond coatings system
The preparation of film rises to 600 DEG C from room temperature with the heating rate of 20 DEG C/min, and keeps the temperature 15min；It is total that gas is controlled in reaction process
Flow is 420mL/min, and methane+argon gas+hydrogen total flow is 420mL/min, wherein methane 15mL/min, argon gas 255mL/
Min, hydrogen 150mL/min.Pressure is 1500Pa.Upper heat extraction silk from metal mesh in metal mesh deposition of diamond coatings device away from
From 25mm, lower heat extraction silk metal mesh distance 15mm in metal mesh deposition of diamond coatings device, sedimentation time is 1.5 hours.
Embodiment 4
A kind of preparation method of diamond coatings metal mesh, comprising the following steps:
(1) metal net surface is cleaned, is cleaned by ultrasonic 2 times using deionized water first, 5 minutes every time, is finally used
Alcohol is cleaned by ultrasonic 10 minutes, with being dried with nitrogen.
(2) corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, and improve diamond nano-particles
Adsorption density.Corrosion treatment is to be cleaned by ultrasonic in aqueous slkali 5 minutes, is then cleaned 30 seconds in acid solution.Wherein aqueous slkali
Are as follows: the NaOH of 1M, acid solution are the HCl of 1M.
(3) metal mesh is cleaned, the etchant solution remained in metal mesh is cleaned up.It is super using deionized water
Sound cleans 2 times, 5 minutes every time, is finally cleaned by ultrasonic 10 minutes with alcohol, with being dried with nitrogen.
(4) the plant crystalline substance for carrying out Nano diamond to metal mesh is handled, and planting brilliant solution is detonation nanodiamond suspension.It plants
Crystal type is to be put into sample in the brilliant solution of plant ultrasound 20 minutes, is taken out, with being dried with nitrogen.
(5) three-dimensional manometer thin diamond is carried out to the metal mesh after planting crystalline substance using metal mesh deposition of diamond coatings system
The preparation of film rises to 500 DEG C from room temperature with the heating rate of 15 DEG C/min, and keeps the temperature 20min；It is total that gas is controlled in reaction process
Flow is 500mL/min, and methane+argon gas+hydrogen total flow is 500mL/min, wherein methane 5mL/min, argon gas 255mL/
Min, hydrogen 140mL/min.Pressure is 2000Pa.Upper heat extraction silk from metal mesh in metal mesh deposition of diamond coatings device away from
From 25mm, lower heat extraction silk metal mesh distance 15mm in metal mesh deposition of diamond coatings device, sedimentation time is 4 hours.
Embodiment 5
A kind of preparation method of diamond coatings metal mesh, comprising the following steps:
(1) metal net surface is cleaned, is cleaned by ultrasonic 2 times using deionized water first, 5 minutes every time, is finally used
Alcohol is cleaned by ultrasonic 5 minutes, with being dried with nitrogen.
(2) corrosion treatment is carried out to cleaned metal mesh, increases surface roughness, and improve diamond nano-particles
Adsorption density.Corrosion treatment is to be cleaned by ultrasonic in aqueous slkali 5 minutes, is then cleaned 30 seconds in acid solution.Wherein aqueous slkali
Are as follows: the NaOH of 1M, acid solution are the HCl of 1M.
(3) metal mesh is cleaned, the etchant solution remained in metal mesh is cleaned up.It is super using deionized water
Sound cleans 2 times, 5 minutes every time, is finally cleaned by ultrasonic 5 minutes with alcohol, with being dried with nitrogen.
(4) the plant crystalline substance for carrying out Nano diamond to metal mesh is handled, and planting brilliant solution is detonation nanodiamond suspension.It plants
Crystal type is to be put into sample in the brilliant solution of plant ultrasound 60 minutes, is taken out, with being dried with nitrogen.
(5) three-dimensional manometer thin diamond is carried out to the metal mesh after planting crystalline substance using metal mesh deposition of diamond coatings system
The preparation of film rises to 800 DEG C from room temperature with the heating rate of 25 DEG C/min, and keeps the temperature 10min；It is total that gas is controlled in reaction process
Flow is 500mL/min, and methane+argon gas+hydrogen total flow is 500mL/min, wherein methane 5mL/min, argon gas 255mL/
Min, hydrogen 140mL/min.Pressure is 1500Pa.Upper heat extraction silk from metal mesh in metal mesh deposition of diamond coatings device away from
From 20mm, lower heat extraction silk metal mesh distance 18mm in metal mesh deposition of diamond coatings device, sedimentation time is 2 hours.
Comparative example 1
A kind of preparation method of diamond coatings metal mesh, unlike the first embodiment, step (5) metal mesh deposition gold
Metal mesh deposition of diamond coatings device is free of in hard rock coat system, and metal mesh is directly placed in substrate location, makes row
Heated filament is from metal mesh distance 25mm, and lower heat extraction silk is from metal mesh distance 15mm.
Comparative example 2
A kind of preparation method of diamond coatings metal mesh, unlike the first embodiment, step (5) using microwave etc. from
Daughter CVD method carries out the preparation of three-dimensional manometer diamond thin to the metal mesh after planting crystalline substance, and experiment condition: reaction gas is total
Flow is 300sccm, ratio H2: CH4=292:8 (sccm), pressure 130Torr, microwave power 1.7kw, deposition substrate temperature
About 800 DEG C, sedimentation time 7h of degree, obtaining diamond film thickness is about 2 μm.
Comparative example 3
A kind of preparation method of diamond coatings metal mesh, unlike the first embodiment, step (5) utilize flame combustion
Method carries out the preparation of three-dimensional manometer diamond thin to the metal mesh after planting crystalline substance, experiment condition: reaction gas total flow is
500sccm, ratio H2: C2H2: O2=5:245:250 (sccm), pressure 1000Pa, deposition substrate temperature are about 1000 DEG C,
Sedimentation time is 5h, and obtaining diamond film thickness is about 2 μm.
Test example
The diamond coatings metal mesh obtained with contact angle measurement measurement embodiment 1, the diamond coatings metal netlist
Face is in air environment to the contact angle of 3 microlitres of n-hexane less than 120, it is super hydrophobic material；Again by diamond coatings metal
Net is immersed in n-hexane, and measurement metal net surface is greater than 140 to the contact angle of 3 microlitres of water0, it is lipophilic material.
In order to investigate the water-oil separating performance for the diamond coatings metal mesh that embodiment and comparative example obtains, grease point is carried out
From efficiency and service life, test method is as follows:
(1) water-oil separating efficiency: obtained metal mesh being placed among the filter being disposed vertically and fixed with clip,
By n-hexane and water, 1:2 obtains oil water mixture under the conditions of magnetic agitation in proportion, and filtering is poured into the import for pouring into part
In device, the n-hexane in mixture is quickly through metal mesh, and the top that water is blocked in metal mesh cannot pass through, and realizes grease
Separation, by calculating the weight for being retained in water above metal mesh and the original ratio for pouring into the weight of water in oil water mixture,
Obtain separative efficiency.
(2) service life: obtained metal mesh is repeated according to above-mentioned oil-water separation test using after each use
Wash with water it is clean, using calculating separative efficiency after 50 times.
Test result is as shown in table 1.
Table 1
| Embodiment or comparative example | Water-oil separating efficiency % | Separative efficiency % after reusing 50 times |
| Embodiment 1 | 99.4 | 99.2 |
| Embodiment 2 | 99.6 | 99.3 |
| Embodiment 3 | 99.7 | 99.2 |
| Embodiment 4 | 99.3 | 99.0 |
| Embodiment 5 | 99.8 | 99.4 |
| Comparative example 1 | 95.8 | 91.4 |
| Comparative example 2 | 97.5 | 92.8 |
| Comparative example 3 | 86.6 | 75.4 |
From the results shown in Table 1, embodiment 1-5 by using the utility model metal mesh deposition of diamond coatings
The metal mesh water-oil separating that system and device obtain is high-efficient, and up to 99% or more, and after recycling 50 times, separative efficiency is almost
It remains unchanged, this shows that the metal mesh of preparation has excellent recuperability, long service life.
Comparative example 1 is not fixed metal mesh using the fixture of metal mesh deposition of diamond coatings device, obtains
Metal mesh water-oil separating performance is declined, this is because metal mesh has slight deformation during the deposition process at high temperature, is caused
The depositing temperature of each point is different on metal mesh, and film growth is uneven, influences its water-oil separating performance.
Comparative example 2 carries out Diamond coating deposition using microwave plasma CVD method, and depositing temperature is high, depositing device
Valuableness, it is at high cost, and can only on small size workpiece long diamond thin, and the metal mesh of water-oil separating is all large area
, therefore this method is only suitable for laboratory research in metal net surface depositing diamond film, is not suitable for industrialized production and a large amount of
Industrial use.
Comparative example 3 carries out Diamond coating deposition using flame combustion process, and the oil-water separation of obtained metal mesh is not
Good, this is because flame combustion process depositing temperature is high, the diamond thin grown on metal mesh is uneven, influences its water-oil separating
Performance.
Although illustrate and describing the utility model with specific embodiment, it will be appreciated that without departing substantially from this reality
Many other change and modification can be made in the case where novel spirit and scope.It is, therefore, intended that in appended right
It include all such changes and modifications belonged in the scope of the utility model in it is required that.
Claims (10)
1. a kind of metal mesh deposition of diamond coatings device, which is characterized in that the metal mesh deposition of diamond coatings device packet
Include chuck body (100)；
The chuck body (100) includes the first noumenon disposed in parallel (110) and the second ontology (120), the first noumenon
(110) and the body interior of second ontology (120) independently has cavity, and metal mesh (200) is placed in the first
Between body (110) and second ontology (120), and metal mesh (200) marginal dimension is greater than the first noumenon (110) and institute
The pore size of the second ontology (120) is stated, the first noumenon (110) is with second ontology (120) by perpendicular to described
The detachable clamp system (130) of the first noumenon (110) is fixed, to clamp the first noumenon (110) and second ontology
(120) metal mesh (200) between.
2. metal mesh deposition of diamond coatings device described in accordance with the claim 1, which is characterized in that the first noumenon
(110) and second ontology (120) is molybdenum disk.
3. metal mesh deposition of diamond coatings device described in accordance with the claim 1, which is characterized in that the detachable clamping machine
Structure (130) includes bolt (131) and nut (132).
4. according to the described in any item metal mesh deposition of diamond coatings devices of claim 1-3, which is characterized in that the fixture
Ontology (100) further includes the first spring leaf (141) or second spring piece (142)；
First spring leaf (141) is located on the inside of the first noumenon (110)；
Second spring piece (142) is located on the inside of second ontology (120).
5. according to the described in any item metal mesh deposition of diamond coatings devices of claim 1-3, which is characterized in that the fixture
Ontology (100) further includes the first spring leaf (141) and second spring piece (142)；
First spring leaf (141) is located on the inside of the first noumenon (110)；
The second spring piece (142) is located on the inside of second ontology (120).
6. including the metal mesh depositing diamond painting of the described in any item metal mesh deposition of diamond coatings devices of claim 1-5
Layer system.
7. metal mesh deposition of diamond coatings system according to claim 6, which is characterized in that the metal mesh deposition gold
Hard rock coat system includes vacuum system and the reaction chamber that is connected with the vacuum system；
Hot wire heater (300) are equipped in the reaction chamber；The hot wire heater includes upper and lower heat extraction silk；The metal mesh is heavy
Product diamond coatings device is as between upper and lower heat extraction silk.
8. metal mesh deposition of diamond coatings system according to claim 7, which is characterized in that the hot wire heater
(300) top is equipped with gas distributor；
The gas distributor includes hydrogen chamber, methane gas chamber and water cooling chamber；The hydrogen chamber is equipped with hydrogen paths, for being passed through
Hydrogen；The methane gas chamber is equipped with methane channel, for being passed through methane gas；The water cooling chamber is equipped with inlet and outlet,
For being passed through cooling water.
9. according to metal mesh deposition of diamond coatings system described in claim 7 or 8, which is characterized in that the heated filament heating
The heated filament of device (300) is tungsten wire；
The tungsten wire diameter is 1-3mm.
10. according to metal mesh deposition of diamond coatings system described in claim 7 or 8, which is characterized in that the heat extraction up and down
Vertical range between silk is 30-40mm；
Wherein, vertical range of the upper heat extraction flight lead from metal mesh (200) is 20-25mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257799A (en) * | 2018-03-12 | 2019-09-20 | 深圳先进技术研究院 | Preparation method, metal mesh depositing coating device, diamond coatings metal mesh and its application of water-oil separating diamond coatings metal mesh |
| CN115266850A (en) * | 2022-07-26 | 2022-11-01 | 长春工业大学 | A kind of preparation method of aptamer sensor for detecting cefquinol |
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2018
- 2018-03-12 CN CN201820338175.7U patent/CN208346252U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257799A (en) * | 2018-03-12 | 2019-09-20 | 深圳先进技术研究院 | Preparation method, metal mesh depositing coating device, diamond coatings metal mesh and its application of water-oil separating diamond coatings metal mesh |
| CN110257799B (en) * | 2018-03-12 | 2024-10-22 | 深圳先进技术研究院 | Preparation method of oil-water separation diamond coating metal net, metal net deposition coating device, diamond coating metal net and application thereof |
| CN115266850A (en) * | 2022-07-26 | 2022-11-01 | 长春工业大学 | A kind of preparation method of aptamer sensor for detecting cefquinol |
| CN115266850B (en) * | 2022-07-26 | 2024-04-12 | 长春工业大学 | A preparation method of aptamer sensor for detecting cefquinome |
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