CN106222718A - A kind of electro-deposition method of carboxymethyl cellulose - Google Patents
A kind of electro-deposition method of carboxymethyl cellulose Download PDFInfo
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Abstract
The present invention relates to the electro-deposition method of a kind of carboxymethyl cellulose.The electro-deposition method of a kind of carboxymethyl cellulose, it is characterised in that it comprises the steps: 1) preparation carboxymethyl cellulose electrodeposit liquid；2) preparation of metal electrode material: use metallic copper or metallic cobalt as the anode metal material of carboxymethyl cellulose electro-deposition, use platinized platinum as the cathodic metal material of carboxymethyl cellulose electro-deposition；3) electro-deposition of carboxymethyl cellulose: anode and negative electrode are contemporaneously immersed in the container equipped with carboxymethyl cellulose electrodeposit liquid, and anode and negative electrode are connected to DC source, carry out the electro-deposition of carboxymethyl cellulose, sedimentation time is 3～10 minutes, obtains being electrodeposited in the carboxymethyl cellulose deposition layer of anode metal electrodes material surface.The method can form carboxymethyl cellulose deposition layer at metal electrode substrates, have that preparation condition is gentle, simple to operation, easily controllable, instrument and equipment simple, environmental protection, favorable repeatability, advantage with low cost.
Description
Technical field
The invention belongs to the fields such as macromolecular material, biological macromolecule material, electrochemistry, Coordinative Chemistry, particularly relate to
A kind of electro-deposition method of carboxymethyl cellulose.
Background technology
Electro-deposition techniques can provide simply and easily, controlled method causes big point of the biology with stimulating responsive
Son assembling, and on metal electrode formed sedimentary [Biosensors and Bioelectronics, 2016,80:222-
229].Conducting polymer thin film, biological devices, biomacromolecule gel etc. can be built, it is also possible to logical by electro-deposition techniques
The method crossing codeposition realizes the assembling [Polymers, 2015,7:1-46] on electrode such as nano material, biological substance.Electricity
Deposition technique possesses accurate space time selectivity and controllability, and Simultaneous Electrodeposition technology has simple to operate, mild condition,
Utilize this technology can realize multiple biomacromolecule in different types of electrode and substrate surface electro-deposition, therefore pass at biology
The field such as sensor, drug release has a good application prospect.
Biomacromolecule is extensively stored in nature in animals and plants and microorganism, with the macromolecular material phase of chemosynthesis
Ratio, biomacromolecule has extensive, the good biocompatibility of a lot of performance characteristics and advantage, such as material source, biological fall
Xie Xing, environment friendly and recyclability etc.；And have in many biomacromolecules containing some reaction active groups (such as carboxylic
The groups such as base, amino and hydroxyl), therefore can be modified preparing the material of different demand by methods such as chemistry, physics
Material.Carboxymethyl cellulose is a kind of water soluble anion polysaccharide [Carbohydrate to human non-toxic's side effect
Polymers, 2014,112:32-38], also it is currently used widest in area, cellulose derivative that consumption is maximum；Carboxymethyl is fine
Dimension element be white or micro-yellow fibers element powder, have odorless, tasteless, nontoxic, be dissolved in the performance characteristics such as water, be widely used
In the material such as biology, medicine, hydrogel, such as film former, adhesive and emulsion stabilizer.It addition, carboxymethyl is fine
Dimension element has stronger coordination ability [Biomacromolecules 2007,8,2762-2767], such as carboxylic first to metal ion
Base cellulose has coordination to copper ion, and its coordination product can separate out the most in the solution, and precipitate is flocculent deposit.
In sum, if it is possible to be directly realized by carboxymethyl cellulose in electro-deposition on the metal material, will build
Biomacromolecule or the gel of natural polymer carboxymethyl derivant, thin film, electrode modified material, biosensor, detector,
The aspects such as bioelectrode have good using value.But, the electro-deposition method about carboxymethyl cellulose has no phase at present
Close document and patent report.
Summary of the invention
The technical problem to be solved in the present invention is: provide the electro-deposition method of a kind of carboxymethyl cellulose, and the method can be
Metal electrode substrates forms carboxymethyl cellulose deposition layer, and can easily take off from surface of metal electrode, also holds
Easily obtain and there is certain thickness carboxymethyl cellulose deposition layer；The method have preparation condition gentle, simple to operation,
Easily controllable, instrument and equipment is simple, environmental protection, favorable repeatability, advantage with low cost.
The present invention solves that the technical scheme that above-mentioned technical problem provides is: the electro-deposition side of a kind of carboxymethyl cellulose
Method, it is characterised in that it comprises the steps:
1) preparation carboxymethyl cellulose electrodeposit liquid: carboxymethyl cellulose powder is added in distilled water and prepare percent mass
Specific concentration is the cmc soln of 1%～3%, carries out magnetic agitation until carboxymethyl cellulose powder at 15～30 DEG C
End is fully dissolved, then by the cmc soln decompression sucking filtration 1 of configuration～2 times (vacuum of decompression sucking filtration is-
0.03MPa～-0.08MPa), remove undissolved carboxymethyl cellulose completely, prepare mass percent concentration be 1%～
The carboxymethyl cellulose electrodeposit liquid of 3%；
2) preparation of metal electrode material (negative electrode and anode): use metallic copper or metallic cobalt as carboxymethyl cellulose electricity
The anode metal material (anode metal material such as difform copper or cobalt sheet metal, tinsel, metal bar) of deposition, first uses sand
Paper to carefully polishing at the surface of anode metal material and the out-of-flatness at edge until flat smooth, then by anode metal material
Ultrasonic cleaning 5 distinguished successively in distilled water, dehydrated alcohol, acetone, distilled water by material～(ultrasonic power was 50-60 in 15 minutes
Watt), then by the ultrasonic cleaning 1～(ultrasonic power was 50-in 3 minutes in the hydrochloric acid solution of 0.5～2.0M of this anode metal material
60 watts), then it is again dipped into ultrasonic cleaning 5～15 minutes (ultrasonic power is 50-60 watt) in distilled water, obtains required sun
Pole metal electrode material, standby；
Use platinized platinum as the cathodic metal material of carboxymethyl cellulose electro-deposition, by platinized platinum successively dehydrated alcohol, third
In ketone, distilled water, difference ultrasonic cleaning 5～15 minutes (ultrasonic power is 50-60 watt), standby；
3) electro-deposition of carboxymethyl cellulose: take step 1) prepared by carboxymethyl cellulose electrodeposit liquid 20～30mL add
Enter in container (such as: small beaker), ultrasonic de-soak 3～5 minutes (ultrasonic power is 50-60 watt)；Then use step 2) in accurate
The anode metal electrodes material (copper or cobalt metal material) got ready is as anode, and cathodic metal material (platinized platinum), will as negative electrode
Anode and negative electrode are contemporaneously immersed in the container (such as: small beaker) equipped with carboxymethyl cellulose electrodeposit liquid, and by anode and the moon
Pole is connected to DC source (high precision DC power supply), and DC source is adjusted to constant voltage mode, and voltage is set to 0.5～1.5V,
Carrying out the electro-deposition of carboxymethyl cellulose, sedimentation time is 3～10 minutes；Electro-deposition closes DC source after terminating, and takes out table
Face electro-deposition has the anode of carboxymethyl cellulose deposition layer, cleans anode surface 5～15 times with distilled water, is electrodeposited in
The carboxymethyl cellulose deposition layer on anode metal electrodes material (copper or cobalt metal material) surface.
The electro-deposition method of a kind of carboxymethyl cellulose of the present invention also connected applications for electronic technology and biotechnology carries
Supplied effective ways and approach, can be applicable to biosensor, detector, chip lab, the modification of biomedical metal material, with
And realize the fields such as the nano material codeposition with biological substance.The electro-deposition method of a kind of carboxymethyl cellulose of the present invention, also
The electricity that can be applied to carry out other biomacromolecule or natural polymer carboxymethyl derivant (such as carboxymethyl chitosan) sinks
Long-pending, have building the aspect such as biomacromolecule or the gel of natural polymer carboxymethyl derivant, thin film, electrode modified material
Good using value.
The know-why of the present invention: containing groups such as carboxyls in the strand of carboxymethyl cellulose, can be with copper ion, cobalt
The metal ion generation coordinations such as ion, form the coordination compound of carboxymethyl cellulose and metal ion.In electro-deposition
Cheng Zhong, after applying voltage on metal electrode, the anode electrochemical oxidation reaction that metal electrode occurs forms metal ion；Such as
When using metallic copper as anode, the electrochemical oxidation reactions of anode forms copper ion, when using metallic cobalt as anode,
The electrochemical oxidation reactions of anode forms cobalt ion；Then these metal ions further with the carboxymethyl cellulose in electrodeposit liquid
There is coordination in element, thus forms carboxymethyl cellulose deposition layer in surface of metal electrode electro-deposition.Present invention profit simultaneously
The electrochemical oxidation reactions occurred with anode can form the metal ion with coordination ability, and carboxymethyl cellulose is permissible
With the feature of metal ion generation coordination, thus the directly electricity realizing carrying out carboxymethyl cellulose on metal electrode is heavy
Long-pending.
The invention has the beneficial effects as follows:
1) the invention provides the electro-deposition method of a kind of carboxymethyl cellulose, the method is to utilize in electrodeposition process,
The electrochemical oxidation reactions that metal electrode occurs at anode can produce metal ion, and these metal ions can be with carboxymethyl cellulose
There is coordination in element, thus realizes carboxymethyl cellulose electro-deposition on metal electrode, is can realizing of a kind of novelty
The method of the direct electro-deposition of carboxymethyl cellulose.
2) electro-deposition method of a kind of carboxymethyl cellulose of the present invention, prepared carboxymethyl cellulose deposition layer outward appearance
Flat smooth, surface bubble-free, and can easily take off from surface of metal electrode, also it is readily available and there is certain thickness carboxylic
Methylcellulose deposition layer.
3) electro-deposition method of a kind of carboxymethyl cellulose of the present invention, the carboxymethyl cellulose used by the method has source
Extensively, good biocompatibility, avirulence, biodegradability, environment friendly and green feature and the advantage such as renewable,
Therefore the application in bio-medical field of the prepared carboxymethyl cellulose electrodeposited material it is advantageous to.
4) electro-deposition method of a kind of carboxymethyl cellulose of the present invention, has that preparation condition is gentle, simple to operate, is prone to control
System, instrument and equipment are simple, favorable repeatability, environmental protection, feature and the advantage such as with low cost, the method be also equipped with space and time
Between the feature such as selectivity and controllability.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 photo at metal copper sheet substrates carboxymethyl cellulose deposition layer.
Fig. 2 is the embodiment of the present invention 2 photo at metal copper wire substrates carboxymethyl cellulose deposition layer.
Fig. 3 be the embodiment of the present invention 3 at metallic cobalt sheet substrates carboxymethyl cellulose deposition layer in 254 nanometer ultraviolets
Fluorescence photo under lamp.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings, and it is right that certain following embodiment should not be construed as
The restriction of the present invention.
The present invention provides the electro-deposition method of a kind of carboxymethyl cellulose, prepares the present invention below in conjunction with specific embodiment
Method is described further, but does not limit the present invention.
Embodiment 1
A kind of electro-deposition method of carboxymethyl cellulose, it comprises the following specific steps that:
1) preparation carboxymethyl cellulose electrodeposit liquid: (chemical reagent is limited from traditional Chinese medicines group by carboxymethyl cellulose powder
Company buys) add that to prepare mass percent concentration in distilled water be the cmc soln of 1%, at 15 DEG C, carry out magnetic
Power stirs until carboxymethyl cellulose powder fully dissolves, then by the cmc soln decompression sucking filtration 1 time of configuration, complete
The undissolved carboxymethyl cellulose of full removal (in order to obtain the cmc soln that mass percent concentration is 1%, is being joined
During cmc soln processed, suitably can add some carboxymethyl cellulose solid samples more), prepare mass percent
Concentration is the carboxymethyl cellulose electrodeposit liquid of 1%；
2) preparation of metal electrode material (negative electrode and anode): use metal copper sheet as carboxymethyl cellulose electro-deposition
Anode metal material, first with sand paper to carefully polishing at the surface of copper sheet and the out-of-flatness at edge until flat smooth, will
Anode metal material after polishing difference ultrasonic cleaning 5 minutes in distilled water, dehydrated alcohol, acetone, distilled water successively, then will
This anode metal material is ultrasonic cleaning 3 minutes in the hydrochloric acid solution of 0.5M, are then again dipped into ultrasonic cleaning 5 points in distilled water
Clock, obtains required anode metal electrodes material, standby；
Use platinized platinum as the cathodic metal material of carboxymethyl cellulose electro-deposition, by platinized platinum successively dehydrated alcohol, third
In ketone, distilled water, difference ultrasonic cleaning 5 minutes, standby；
3) electro-deposition of carboxymethyl cellulose: take step 1) prepared by carboxymethyl cellulose electrodeposit liquid 20mL add little
In beaker, ultrasonic de-soak 3 minutes；Then use step 2) in ready copper sheet as anode, platinized platinum is as negative electrode, by anode
It is contemporaneously immersed in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid with negative electrode, and anode and negative electrode are connected to unidirectional current
Source (high precision DC power supply), DC source is adjusted to constant voltage mode, and voltage is set to 0.5, carries out the electricity of carboxymethyl cellulose
Deposition, sedimentation time is 10 minutes；Electro-deposition closes DC source after terminating, and taking out surface electro-deposition has carboxymethyl cellulose electricity
The copper sheet of sedimentary, carefully cleans anode surface 5 times with distilled water, obtains being electrodeposited in the carboxymethyl cellulose on metal copper sheet surface
Element deposition layer.
Fig. 1 is the embodiment of the present invention 1 photo at metal copper sheet substrates carboxymethyl cellulose deposition layer.By Fig. 1
It is found that when using metal copper sheet as anode metal material, form one layer of obvious carboxylic after electro-deposition on copper sheet surface
Methylcellulose deposition layer, this carboxymethyl cellulose deposition layer is blueness, has certain thickness gel film, flat appearance
Smooth, surface bubble-free, and can easily take off from metallic copper plate electrode surface, film has certain intensity；Above-mentioned knot
Fruit explanation, utilizes the electro-deposition method of a kind of carboxymethyl cellulose of the present invention, can obtain carboxymethyl cellulose on metal copper sheet
Element deposition layer.
Embodiment 2
A kind of electro-deposition method of carboxymethyl cellulose, it comprises the following specific steps that:
1) preparation carboxymethyl cellulose electrodeposit liquid: carboxymethyl cellulose powder is added in distilled water and prepare percent mass
Specific concentration is the cmc soln of 3%, carries out magnetic agitation until carboxymethyl cellulose powder is the most molten at 30 DEG C
Solve, then by the cmc soln decompression sucking filtration 2 times of configuration, remove undissolved carboxymethyl cellulose completely, preparation
Obtain the carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 3%；
2) preparation of metal electrode material (negative electrode and anode): use metal copper wire as carboxymethyl cellulose electro-deposition
Anode metal material, first with sand paper to carefully polishing at the out-of-flatness on the surface of copper wire until flat smooth, will be after polishing
Anode metal material respectively ultrasonic cleaning 15 minutes in distilled water, dehydrated alcohol, acetone, distilled water successively, then by this sun
Pole metal material is ultrasonic cleaning 1 minute in the hydrochloric acid solution of 2.0M, is then again dipped into ultrasonic cleaning 15 minutes in distilled water
Obtain required anode metal electrodes material, standby；
Use platinized platinum as the cathodic metal material of carboxymethyl cellulose electro-deposition, by platinized platinum successively dehydrated alcohol, third
In ketone, distilled water, difference ultrasonic cleaning 15 minutes, standby；
3) electro-deposition of carboxymethyl cellulose: take step 1) prepared by carboxymethyl cellulose electrodeposit liquid 30mL add little
In beaker, ultrasonic de-soak 5 minutes；Then use step 2) in ready copper wire as anode, platinized platinum is as negative electrode, by anode
It is contemporaneously immersed in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid with negative electrode, and anode and negative electrode are connected to unidirectional current
Source (high precision DC power supply), DC source is adjusted to constant voltage mode, and voltage is set to 1.5V, carries out the electricity of carboxymethyl cellulose
Deposition, sedimentation time is 3 minutes；Electro-deposition closes DC source after terminating, and taking out surface electro-deposition has carboxymethyl cellulose electricity
The copper wire of sedimentary, carefully cleans anode surface 15 times with distilled water, and the carboxymethyl obtaining being electrodeposited in metal copper wire surface is fine
Dimension element deposition layer.
Fig. 2 is the embodiment of the present invention 2 photo at metal copper wire substrates carboxymethyl cellulose deposition layer.By Fig. 2
It is found that when use metal copper wire as anode metal material time, define on metal copper wire surface after electro-deposition one layer bright
Aobvious carboxymethyl cellulose deposition layer, this carboxymethyl cellulose deposition layer is blueness, has certain thickness gel film, film
Flat appearance, smooth surface bubble-free；The above results illustrates, utilizes the electro-deposition side of a kind of carboxymethyl cellulose of the present invention
Method, can obtain carboxymethyl cellulose deposition layer on metal copper wire.
Embodiment 3
A kind of electro-deposition method of carboxymethyl cellulose, it comprises the following specific steps that:
1) preparation carboxymethyl cellulose electrodeposit liquid: carboxymethyl cellulose powder is added in distilled water and prepare percent mass
Specific concentration is the cmc soln of 2%, carries out magnetic agitation until carboxymethyl cellulose powder is the most molten at 20 DEG C
Solve, then by the cmc soln decompression sucking filtration 2 times of configuration, remove undissolved carboxymethyl cellulose completely, preparation
Obtain the carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 2%；
2) preparation of metal electrode material (negative electrode and anode): use metallic cobalt sheet as carboxymethyl cellulose electro-deposition
Anode metal material, first with sand paper to carefully polishing at the surface of cobalt sheet and the out-of-flatness at edge until flat smooth, will
Anode metal material after polishing difference ultrasonic cleaning 10 minutes in distilled water, dehydrated alcohol, acetone, distilled water successively, then
By this anode metal material ultrasonic cleaning 2 minutes in the hydrochloric acid solution of 1.0M, then it is again dipped into ultrasonic cleaning in distilled water
Within 10 minutes, obtain required anode metal electrodes material, standby；
Use platinized platinum as the cathodic metal material of carboxymethyl cellulose electro-deposition, by platinized platinum successively dehydrated alcohol, third
In ketone, distilled water, difference ultrasonic cleaning 10 minutes, standby；
3) electro-deposition of carboxymethyl cellulose: take step 1) prepared by carboxymethyl cellulose electrodeposit liquid 25mL add little
In beaker, ultrasonic de-soak 4 minutes；Then use step 2) in ready cobalt metal material as anode, platinized platinum as negative electrode,
Anode and negative electrode are contemporaneously immersed in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid, and anode and negative electrode are connected to
DC source (high precision DC power supply), DC source is adjusted to constant voltage mode, and voltage is set to 1V, carries out carboxymethyl cellulose
Electro-deposition, sedimentation time is 6 minutes；Electro-deposition closes DC source after terminating, and taking out surface electro-deposition has carboxymethyl cellulose
The anode of element deposition layer, carefully cleans anode surface 10 times, obtains being electrodeposited in the carboxylic first on metallic cobalt sheet surface with distilled water
Base cellulose deposition layer.
Fig. 3 be the embodiment of the present invention 3 at metallic cobalt sheet substrates carboxymethyl cellulose deposition layer in 254 nanometer ultraviolets
Fluorescence photo under lamp.The fluorescent staining method of carboxymethyl cellulose deposition layer is: be the carboxylic of 2% at mass percent concentration
Methylcellulose electrodeposit liquid is that 0.1% addition rhodamine 6G carries out fluorescence staining according to mass percent concentration, so that
Fluorescence must be had, then to it under 254 nanometer uviol lamps at the carboxymethyl cellulose deposition layer of metallic cobalt sheet substrates
Fluorescence is observed.By Fig. 3 it is found that when use metallic cobalt sheet as anode metal material time, at metallic cobalt after electro-deposition
Sheet surface defines carboxymethyl cellulose deposition layer, and this carboxymethyl cellulose deposition layer sends under 254 nanometer uviol lamps
Significantly fluorescence, flat appearance, smooth surface bubble-free；Illustrate to utilize the method can be on anode conducting metal material cobalt sheet
Obtain carboxymethyl cellulose deposition layer；The above results illustrates, utilizes the electro-deposition method of a kind of carboxymethyl cellulose of the present invention,
Carboxymethyl cellulose deposition layer can be obtained on metallic cobalt sheet.
It should be noted that it will be understood by those within the art that, technical scheme can be carried out
Amendment or equivalent, without deviating from objective and the scope of technical solution of the present invention, it all should contain the right in the present invention
In the middle of claimed range.
Claims (3)
1. the electro-deposition method of a carboxymethyl cellulose, it is characterised in that it comprises the steps:
1) preparation carboxymethyl cellulose electrodeposit liquid: carboxymethyl cellulose powder is added preparation mass percent in distilled water dense
Degree is the cmc soln of 1%～3%, carries out magnetic agitation until carboxymethyl cellulose powder is abundant at 15～30 DEG C
Dissolving, then reduce pressure sucking filtration 1～2 times by the cmc soln of configuration, removes undissolved carboxymethyl cellulose completely,
Prepare the carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 1%～3%；
2) preparation of metal electrode material: use metallic copper or metallic cobalt as the anode metal material of carboxymethyl cellulose electro-deposition
Material, first with sand paper to carefully polishing at the surface of anode metal material and the out-of-flatness at edge until flat smooth, then will
Anode metal material respectively ultrasonic cleaning 5～15 minutes in distilled water, dehydrated alcohol, acetone, distilled water successively, then by this sun
Pole metal material ultrasonic cleaning 1～3 minutes in the hydrochloric acid solution of 0.5～2.0M, be then again dipped in distilled water ultrasonic clearly
Wash 5～15 minutes, obtain required anode metal electrodes material, standby；
Employing platinized platinum is as the cathodic metal material of carboxymethyl cellulose electro-deposition, by platinized platinum successively in dehydrated alcohol, acetone, steaming
Respectively ultrasonic cleaning 5～15 minutes in distilled water, standby；
3) electro-deposition of carboxymethyl cellulose: take the carboxymethyl cellulose electrodeposit liquid 20～30mL prepared by step 1) and add appearance
In device, ultrasonic de-soak 3～5 minutes；Then use step 2) in ready anode metal electrodes material as anode, negative electrode gold
Anode and negative electrode, as negative electrode, are contemporaneously immersed in the container equipped with carboxymethyl cellulose electrodeposit liquid by genus material, and by sun
Pole and negative electrode are connected to DC source, and DC source is adjusted to constant voltage mode, and voltage is set to 0.5～1.5V, carry out carboxymethyl
The electro-deposition of cellulose, sedimentation time is 3～10 minutes；Electro-deposition closes DC source after terminating, and taking out surface electro-deposition has
The anode of carboxymethyl cellulose deposition layer, cleans anode surface 5～15 times with distilled water, obtains being electrodeposited in anode metal electricity
The carboxymethyl cellulose deposition layer of pole material surface.
The electro-deposition method of a kind of carboxymethyl cellulose the most according to claim 1, it is characterised in that in step 1), subtract
The vacuum of pressure sucking filtration is-0.03MPa～-0.08MPa.
The electro-deposition method of a kind of carboxymethyl cellulose the most according to claim 1, it is characterised in that ultrasonic power is
50-60 watt.
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| CN110462111A (en) * | 2017-03-29 | 2019-11-15 | 古河电气工业株式会社 | Integrally formed body and the composite material, electrical contact terminal and printed wiring board that body is integrally formed with this |
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| CN107236974A (en) * | 2017-06-13 | 2017-10-10 | 合肥聪亨新型建材科技有限公司 | A kind of preparation method of antibiotic property composite material coating |
| CN110596220A (en) * | 2019-09-25 | 2019-12-20 | 武汉理工大学 | Preparation method of quantum dot electrode for simultaneously carrying out fluorescence and electrochemical detection on metal ions |
| CN110904490A (en) * | 2019-11-18 | 2020-03-24 | 武汉大学 | Preparation method of carboxylated cellulose nanofiber hydrogel |
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