CN109338423A - A kind of method that Low-cost electric chemical deposition prepares rare earth metal Tb film - Google Patents
A kind of method that Low-cost electric chemical deposition prepares rare earth metal Tb film Download PDFInfo
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- CN109338423A CN109338423A CN201811192282.4A CN201811192282A CN109338423A CN 109338423 A CN109338423 A CN 109338423A CN 201811192282 A CN201811192282 A CN 201811192282A CN 109338423 A CN109338423 A CN 109338423A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
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Abstract
The present invention relates to a kind of methods that Low-cost electric chemical deposition prepares rare earth metal Tb film, belong to rare earth metal Low-temperature electro-deposition field.A kind of method that Low-cost electric chemical deposition prepares rare earth metal Tb film, it is characterized in that, including following processing steps: lithium nitrate is dissolved in the DMI electrolyte for obtaining lithium nitrate in DMI, the DMI electrolyte of lithium nitrate is placed in electrolytic cell, anhydrous terbium chloride is added thereto again, is stirred in electrolytic cell, is allowed to form uniform system, whole system temperature is controlled at 25~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；In electrodeposition process, anhydrous terbium chloride is added into electrolytic cell at regular intervals, control terbium chloride molar concentration is initial concentration ± 2%.The method of the invention significantly reduces energy consumption and production cost while efficiently preparing rare earth metal Tb film.
Description
Technical field
The present invention relates to a kind of methods that Low-cost electric chemical deposition prepares rare earth metal Tb film, and it is low to belong to rare earth metal
Warm electrodeposition.
Background technique
Rare earth element is known as " industrial vitamin " " industrial monosodium glutamate ", " mother of new material ", excellent with that can not replace
Different magnetic, light, electrical property increase product variety to properties of product are improved, and raising production efficiency plays the role of huge.Due to
Rare-earth action is big, and dosage is few, it has also become the important element of product structure, technical progress of industry of increasing technology content, promote is improved,
It has been widely applied to the fields such as metallurgy, military affairs, petrochemical industry, glass ceramics, agricultural and new material.Particularly, terbium is mainly answered
For the activator of the green powder in three primary colors fluorescent powder, the phosphate matrix activated such as terbium, the silicate substrate of terbium activation, terbium swash
Cerium Mg aluminate matrix living, issues green light under excited state.In addition, in terms of magneto-optic storage material, terbium in recent years
It is the scale that magneto-optic memory technique has reached mass production, with the magnetooptic disc of Tb-Fe noncrystalline membrane development, makees computer storage member
Part, storage capacity improve 10~15 times.Magneto-optic glass, the Faraday rotation glass containing terbium are that manufacture is answered extensively in laser technology
The critical material of rotator, isolator and circulator.Especially terbium dysprosium ferrum magnetostriction alloy develops, and even more opens
The new application of terbium is warded off, terbium dysprosium ferrum magnetostriction alloy is the new material just found the seventies, there is half composition in the alloy
For terbium and dysprosium, holmium is added sometimes, remaining is iron, which is developed first by the U.S. laboratory Hawkeye State A Musi, when terbium dysprosium
When iron magnetostriction alloy is placed in a magnetic field, the variation of size changes greatly than general magnetic material, and this variation can be with
It is achieved some precision machinery movements.Terbium dysprosium ferrum starts to be mainly used for sonar, is widely used to multiple fields at present, from
Fuel injection system, micro- navigates to mechanical actuator, the regulating mechanism of space telescope and aircraft wing tune at Liquid valve control
The fields such as device are saved, therefore strategy metal element terbium is significant.
Currently, metal vacuum thermal reduction and high temperature fused salt electrolysis are that the traditional of rare earth metal Tb makes from technology
The terbium metal of Preparation Method, preparation uses vacuum evaporation deposition or the sputter deposition depositional coating on base material.The above mistake
The disadvantages of journey is there are energy consumption height, and seriously polluted, long flow path, corrosivity is strong, complicated for operation, the high requirements on the equipment.With the energy
Growing tension and environmental issue it is increasingly prominent, how while obtaining high quality rare earth metal Tb film to the maximum extent
It reduces to the pollution of environment and energy saving and easy to operate, becomes focus concerned by people.Electro-deposition method possesses operation side
Just, simple and flexible, it is lower to base material shape need the features such as, obtained extensive research.If can be in room temperature or close to room
Electro-deposition prepares rare earth metal Tb thin-film material under the conditions of temperature, not only easy to operate but also low in cost, reliable and secure.Due to
The activity of rare earth terbium exception, and its oxidation-reduction potential is very negative, in water solution system rare earth terbium ion on the electrode due to
Liberation of hydrogen shielding action can not directly be reduced to rare earth metal Tb, therefore the system of electrodeposit metals terbium is generally nonaqueous solvents.
Ionic liquid has low melting point, low saturated vapour pressure, electrochemical properties as a kind of nonaqueous solvents, also referred to as low temperature molten salt
The properties such as stable, are also widely used in the research of electrochemistry metallurgical process.But the synthesis technology of ionic liquid is complicated, exchange reaction
It is not thorough, there are competitive reactions and by-product, and products therefrom needs more purification and separation, and this dramatically increases ionic liquids
A possibility that production cost and environmental pollution, reduces the green characteristic of ionic liquid.And last ionic liquid obtained produces
Water content not can guarantee in product, seriously affect ionic liquid electrodeposition preparation active metal terbium membrane process.On the other hand, conventional
Ionic liquid electrochemical window is relatively narrow and limited to general chloride (such as magnesium chloride, calcium chloride, rare earth chloride etc.) solvability,
And some common ion liquid viscosities are big, hygroscopic in air, therefore largely limit the practical application of ionic liquid.
Therefore, at present, ionic liquid develops one-hundred-year history, but is limited only to scientific research in metal electrodeposition field, has no big
Scale actual application background.
Summary of the invention
For above-mentioned existing problem, the present invention provides one kind with lithium nitrate (purity is greater than 99.9%) as supporting electrolyte
Utilize novel non-proton intensive polar solvent 1,3- dimethyl-2-imidazolinone (DMI) (purity is greater than 99.0%) low-temperature electrolytic chlorine
Change the method that terbium prepares terbium metal film.With terbium chloride (purity be not less than 99.9%) for raw material, be dissolved in containing 0.02~
Electro-deposition prepares the Short flow method of high pure metal terbium film in the DMI solvent of 0.1mol/L lithium nitrate, is efficiently preparing rare earth
Energy consumption and production cost are significantly reduced while terbium metal film.
A kind of method that Low-cost electric chemical deposition prepares rare earth metal Tb film, the method is electrodeposition process, including
Following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L,
The DMI electrolyte of lithium nitrate is obtained, the DMI is that structural formula is as follows:
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous terbium chloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form uniform system, wherein terbium chloride molar concentration is 0.01~0.05mol/L, controls whole system temperature
Degree is at 25~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous terbium chloride into electrolytic cell at regular intervals, controls terbium chloride molar concentration
For initial concentration ± 2%.
In above-mentioned technical proposal, the lithium nitrate, terbium chloride purity be not less than 99.9%；The DMI purity is not small
In 99.0%.
" control terbium chloride molar concentration is initial concentration ± 2% " of the present invention refers to that control terbium chloride molar concentration is
The 98%~102% of initial concentration.
" vs Ag " refers to using silver electrode as reference electricity in " decomposition voltage range -2.0~-2.4V vs Ag " of the present invention
Pole.
Preferably, in the step S1, molar concentration of the lithium nitrate in DMI is 0.02~0.1mol/L.
Preferably, in the step S2, terbium chloride molar concentration is 0.02~0.05mol/L.
Preferably, the step S3 adds anhydrous terbium chloride into electrolytic cell every 30min, and control terbium chloride mole is dense
Degree is near initial concentration.
Preferably, the method includes the steps S4, every the terbium metal film associated basis that 60min will be formed in cathode substrate
Bottom material is sealed up for safekeeping in the vessel equipped with dimethyl carbonate or kerosene.
Preferably, the electrolytic process with high-purity leaf (purity >=99.99%) be anode, with pure copper sheet (purity >=
99.99%) or fine aluminium piece (purity >=99.9%) is cathode.
Preferably, the interpolar between the anode and cathode is away from for 15mm.
With it is existing prepare terbium metal film process compared with, the method for the invention has the advantage that
(1) process flow is shortened, and significantly reduces production energy consumption, reduces production cost, improves operating environment, simple and flexible；
(2) the novel non-proton intensive polar solvent electro-deposition of low temperature is used, can reduce and eliminate using high temperature fused salt electrolysis matter
When the shortcomings that energy consumption is high, temperature is high, equipment seriously corroded, easy to operate, furthermore DMI solvent not only possesses terbium chloride excellent molten
Solution property and high dielectric constant also have nontoxic, good chemical and thermal stability, do not corrode to copper and iron, higher boiling, high-flash,
Low melting point easily recycles, the characteristics of having a safety feature.Importantly, DMI solvent possesses extensive chemical industry production background, cost compared with
Molten salt system and ionic liquid are greatly reduced, and in addition DMI can be synthesized with waste plastics and GHG carbon dioxide, green speciality
Obviously, there is large-scale application ability and prospect.Method and process of the invention electro-deposition can prepare rare earth metal at low temperature
Terbium film, obtained product purity is high, lower to equipment requirement, is produced on a large scale to improve efficiency and yield, for low cost
The preparation of rare earth metal green technological reserve and theories integration are provided.
Detailed description of the invention
Fig. 1 is to scheme in embodiment 8 in copper cathode sheets products therefrom SEM.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
The anhydrous terbium chloride purity 99.9% used in the embodiment of the present invention, lithium nitrate purity 99.9%, DMI purity
99.0%.
Using Shanghai Chen Hua electrochemical workstation as electrolysis power in the embodiment of the present invention.
Anode of the embodiment of the present invention is high-purity leaf (purity >=99.9%), annode area 1cm2, cathode is high purity copper
Piece (purity >=99.99%) or aluminium flake (purity >=99.99%), cathode area 1cm2, reference electrode be filamentary silver (purity >=
99.99%, diameter 0.05cm).
The content of terbium element is examined using ICP (inductively coupled plasma atomic emission spectrum) in the embodiment of the present invention
It surveys；Film thickness means of testing is SEM (scanning electron microscope).
The method that Low-cost electric chemical deposition prepares rare earth metal Tb film described in following embodiments, the method are electricity
Sedimentation, including following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L,
Obtain the DMI electrolyte of lithium nitrate；
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous terbium chloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form transparent and homogeneous system, wherein terbium chloride molar concentration is 0.01~0.05mol/L, controls entire body
It is temperature at 25~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous terbium chloride into electrolytic cell at regular intervals, controls terbium chloride molar concentration
For initial concentration ± 2%.
Embodiment 1
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.01mol/L and 0.01mol/L.Control electrolyte system constant temperature 25
DEG C, decomposition voltage is -2.0V (vs Ag), and cathode material is high-purity aluminium flake；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.01mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization, knot
Fruit shows that terbium metal can be effectively deposited and comes out that it is 76.62% that ICP, which detects terbium element total content, observes gained deposition through SEM
Film be even compact deposition film, 0.27 micron of terbium film thickness.
Embodiment 2
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.02mol/L and 0.02mol/L.Control electrolyte system constant temperature 35
DEG C, decomposition voltage is -2.1V (vs Ag), and cathode material is high-purity copper sheet；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.02mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization, knot
Fruit shows that terbium metal can be effectively deposited and comes out that it is 97.47% that ICP, which detects terbium element total content, observes gained deposition through SEM
Film be even compact deposition film, 0.23 micron of terbium film thickness.
Embodiment 3
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.03mol/L and 0.03mol/L.Control electrolyte system constant temperature 45
DEG C, decomposition voltage is -2.2V (vs Ag), and cathode material is high-purity aluminium flake；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.03mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization, knot
Fruit shows that terbium metal can be effectively deposited and comes out that it is 97.74% that ICP, which detects terbium element total content, observes gained deposition through SEM
Film be even compact deposition film, 0.26 micron of terbium film thickness.
Embodiment 4
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.04mol/L and 0.04mol/L.Control electrolyte system constant temperature 55
DEG C, decomposition voltage is -2.3V (vs Ag), and cathode material is high-purity copper sheet；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.04mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization, knot
Fruit shows that terbium metal can be effectively deposited and comes out that it is 99.75% that ICP, which detects terbium element total content, observes gained deposition through SEM
Film be even compact deposition film, 0.33 micron of terbium film thickness.
Embodiment 5
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.05mol/L and 0.06mol/L.Control electrolyte system constant temperature 65
DEG C, decomposition voltage is -2.4V (vs Ag), and cathode material is high-purity aluminium flake；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.05mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization, knot
Fruit shows that terbium metal can be effectively deposited and comes out that it is 99.52% that ICP, which detects terbium element total content, observes gained deposition through SEM
Film be even compact deposition film, 0.36 micron of terbium film thickness.
Embodiment 6
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.025mol/L and 0.08mol/L.Control electrolyte system constant temperature 75
DEG C, decomposition voltage is -2.4V (vs Ag), and cathode material is high-purity copper sheet；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.025mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization,
It is come out the result shows that terbium metal can be effectively deposited, it is 99.61% that ICP, which detects terbium element total content, is swept SEM observation gained
Deposition film be even compact deposition film, 0.37 micron of terbium film thickness.
Embodiment 7
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.035mol/L and 0.1mol/L.Control electrolyte system constant temperature 80
DEG C, decomposition voltage is -2.3V (vs Ag), and cathode material is high-purity aluminium flake；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.035mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization,
It is come out the result shows that terbium metal can be effectively deposited, it is 99.74% that ICP, which detects terbium element total content, heavy through SEM observation gained
Product film be even compact deposition film, 0.43 micron of terbium film thickness.
Embodiment 8
Preparing electrolyte raw material is terbium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein terbium chloride and lithium nitrate molar concentration are respectively 0.015mol/L and 0.1mol/L.Control electrolyte system constant temperature 55
DEG C, decomposition voltage is -2.3V (vs Ag), and cathode material is high-purity copper sheet；It carries out once adding terbium chloride operation after being electrolysed 30min
Make system terbium chloride concentration 0.015mol/L；It is electrolysed after 60min and saves substrate together with deposit collection.It is detected through characterization,
It is come out the result shows that terbium metal can be effectively deposited, it is 99.98% that ICP, which detects terbium element total content, heavy through SEM observation gained
Product film be even compact deposition film, 0.46 micron of terbium film thickness.
Claims (7)
1. a kind of method that Low-cost electric chemical deposition prepares rare earth metal Tb film, it is characterised in that: the method is that electricity is heavy
Area method, including following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L, is obtained
The DMI electrolyte of lithium nitrate, the DMI are that structural formula is as follows:
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous terbium chloride is added thereto by S2, stirs in electrolytic cell
Mixing, is allowed to form uniform system, and wherein terbium chloride molar concentration is 0.01~0.05mol/L, and control whole system temperature exists
25~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrodeposition process, adds anhydrous terbium chloride into electrolytic cell at regular intervals, and control terbium chloride molar concentration is
Initial concentration ± 2%.
2. according to the method described in claim 1, it is characterized by: in the step S1, molar concentration of the lithium nitrate in DMI
For 0.02~0.1mol/L.
3. according to the method described in claim 1, it is characterized by: in the step S2, terbium chloride molar concentration is 0.02~
0.05mol/L。
4. according to the method described in claim 1, it is characterized by: the step S3, adds nothing into electrolytic cell every 30min
Water terbium chloride, control terbium chloride molar concentration are initial concentration ± 2%.
5. according to the method described in claim 1, it is characterized by: the method includes the steps S4, every 60min by cathode base
In closing vessel of the related base material of terbium metal film formed on bottom equipped with dimethyl carbonate or kerosene.
6. according to the method described in claim 1, it is characterized by: the electrolytic process using high-purity leaf as anode, with fine copper
Piece or fine aluminium piece are cathode.
7. according to the method described in claim 6, it is characterized by: interpolar between the anode and cathode is away from for 15mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811192282.4A CN109338423B (en) | 2018-10-12 | 2018-10-12 | Method for preparing rare earth metal terbium film by low-cost electrochemical deposition |
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| CN201811192282.4A CN109338423B (en) | 2018-10-12 | 2018-10-12 | Method for preparing rare earth metal terbium film by low-cost electrochemical deposition |
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| CN112176372A (en) * | 2020-09-27 | 2021-01-05 | 东北大学 | Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials |
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| CN112176372A (en) * | 2020-09-27 | 2021-01-05 | 东北大学 | Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials |
| CN112176372B (en) * | 2020-09-27 | 2021-10-15 | 东北大学 | Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials |
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