CN107805761A - Iron-nickel alloy paper tinsel and its manufacture method - Google Patents

Iron-nickel alloy paper tinsel and its manufacture method Download PDF

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Publication number
CN107805761A
CN107805761A CN201710795285.6A CN201710795285A CN107805761A CN 107805761 A CN107805761 A CN 107805761A CN 201710795285 A CN201710795285 A CN 201710795285A CN 107805761 A CN107805761 A CN 107805761A
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iron
alloy foil
nickel alloy
nickel
face
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CN107805761B (en
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金锺权
郑官颢
金县泰
李载坤
梁洪硕
金基洙
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Posco Holdings Inc
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Posco Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Electroluminescent Light Sources (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Cell Electrode Carriers And Collectors (AREA)

Abstract

The present invention relates to iron nickel (Fe Ni) Alloy Foil, more specifically, is related to iron-nickel alloy paper tinsel and its manufacture method that one kind is suitable for Organic Light Emitting Diode (OLED) material.

Description

Iron-nickel alloy foil and its manufacture method
Technical field
The present invention relates to iron-nickel (Fe-Ni) Alloy Foil, more specifically, it is related to one kind and is suitable for organic light-emitting diodes Manage the iron-nickel alloy foil and its manufacture method of (OLED) material.
Background technology
Organic Light Emitting Diode (Organic Light Emitting Diode, OLED) is in current display device market Attracted tremendous attention as the display device of new generation that can substitute LCD (Liquid Crystal Display, liquid crystal display).
OLED can voluntarily send light and color, adjust the amount of light, have little power consumption, fast response time, almost without image retention The advantages of.In addition, color sensation is true to nature bright, visual field angular width.
Due to this advantage, OLED display industry is just being directed to automobile, mobile device and TV markets recently.
Manufacture the full color (Full being made up of RGB sub-pixels (RGB Sub-Pixel) used during OLED display Color) element is made in the evaporated device of high temperature.The evaporated device is made up of substrate, deposition mask, framework etc., Because evaporation process is carried out at high temperature, thus it is affected by temperature, sent out due to change in size caused by thermal coefficient of expansion Raw position difference.Accordingly, there exist the position for the deposition material being attached on substrate, precision size degree is low the problem of.So it is The correct position control of mask, the precision for preventing thermal expansion and meeting mask and substrate, it is necessary to select hot swollen with substrate The mask and frame material of swollen coefficient peer-level.
On the other hand, the material as the deposition mask, mainly using the invar alloy of iron-nickel (Fe-Ni) alloy system (Fe-36%Ni).The invar alloy manufactured by existing rolling (rolling) process, in surface roughness control (raised, hole Hole) and thickness control in terms of have difficulties, accordingly, there exist the characteristic of element is low, the problem of manufacture yield significantly reduces.Not only In this way, when manufacturing very thin product (less than 18 μm), the shortcomings that surface caused by impurity being present is bad and manufacturing expense rises.
Thermal coefficient of expansion state thus by the iron-nickel alloy foil of rolling process manufacture is as shown in Figure 1.
Therefore, as the method that can substitute rolling process, iron-nickel is manufactured by electrocasting (electroforming) and closed Goldleaf.
Electrocasting be a kind of rotation set by feed flow nozzle into by electrolytic cell cylindrical cathode drum and it is right therewith The gap that the anode for a pair of the circular shapes put surrounds supplies electrolyte and is passed through electric current, so that Fe-Ni systems alloy is described The surface electro-deposition of cathode drum, the method batched and metal foil is made.The Fe-Ni systems manufactured according to this electrocasting close Golden metal foil has the advantages of average crystal grain size is fine, mechanical properties are excellent, moreover, just can be made with cheap manufacturing expense Make, there is the advantages of manufacturing cost is low.
But it was found that iron-nickel alloy foil is manufactured even from electrocasting, according to the crystalline texture of the Alloy Foil, heat The coefficient of expansion greatly changes, and there is also the low possibility of OLED product properties.
Therefore, when manufacturing iron-nickel alloy foil according to electrocasting, it is desirable to which manufacture is a kind of to be had and can reduce thermal coefficient of expansion Crystalline texture OLED iron-nickel alloy foils.
Prior art literature
Patent document
Patent document 1：KR published patent the 2016-0077575th
The content of the invention
One aspect of the present invention is for providing OLED iron-nickel alloy foils, it is desirable to provide one kind can be by with spy Determine crystalline texture and effectively reduce the iron-nickel alloy foil of thermal coefficient of expansion and manufacture its method.
One aspect of the present invention provides a kind of iron-nickel alloy foil, it is characterised in that is the iron-nickel manufactured with electrocasting Alloy Foil,
The content of nickel is 36~45 weight %, and remaining includes iron (Fe) and inevitable impurity,
The Alloy Foil is organized as face-centred cubic structure (FCC, Face-Centered Cubic), (111) face and (200) the texture coefficient sum in face relative to (111) face, (200) face, (220) face texture coefficient (Texture Coefficient the ratio of summation) is 80~98%, and the ratio of the texture coefficient in (111) face is 60~78%, (200) face The ratio of texture coefficient be 20~30%, the ratio of the texture coefficient in (220) face is less than 20% (including 0%).
Another aspect of the present invention provides a kind of manufacture method of iron-nickel alloy foil, it is characterised in that is utilized comprising iron The method that the electrolyte of compound and nickel compound manufactures iron-nickel alloy foil with electrocasting, iron ion and nickel in the electrolyte The relation of ion represents with following [mathematical expressions 1], the f_Ni of following [mathematical expressions 1]2+Value meets 72~78.
[mathematical expression 1]
f_Ni2+={ [Ni2+]/([Ni2+]+[Fe2+])}×100
(wherein, Ni2+And Fe2+Refer to nickel ion concentration and iron concentration in electrolyte.)
According to the present invention, for the iron-nickel alloy foil manufactured by electrocasting, can provide one kind can be by described The control of the crystalline texture of iron-nickel alloy foil and effectively reduce the iron-nickel alloy foil of thermal coefficient of expansion, this have can be compatibly Effect as OLED materials.
Brief description of the drawings
Fig. 1 is represented with the chart of the thermal coefficient of expansion state of the iron-nickel alloy foil of conventional art (rolling) manufacture.
Fig. 2 is represented with the chart of the thermal coefficient of expansion state of the iron-nickel alloy foil of electrocasting manufacture.(●：With FCC The iron-nickel alloy foil (example) of structure, ■：Iron-nickel alloy foil (comparative example) with FCC+BCC structures).
Fig. 3 illustrates the X-ray diffraction analysis knot of the iron-nickel alloy foil with FCC configuration of one embodiment of the invention Fruit.
Fig. 4 illustrates the X-ray diffraction point of the iron-nickel alloy foil with FCC+BCC structures of one embodiment of the invention Analyse result.
Embodiment
The present inventor provide using electrocasting (electroforming) manufacture iron-nickel (Fe-Ni) Alloy Foil in terms of, The scheme of thermal coefficient of expansion for that can reduce the iron-nickel alloy foil has made intensive studies.Its results verification iron-nickel The thermal coefficient of expansion of Alloy Foil changes with the crystalline texture that the iron-nickel alloy foil has.
Therefore, the present invention has in terms of the iron-nickel alloy foil with the crystalline texture that can reduce thermal coefficient of expansion is provided There is technical meaning.
The present invention is described in detail below.
Iron-nickel (Fe-Ni) Alloy Foil of one aspect of the invention is manufactured with electrocasting, and preferably the content of nickel is 36~45 weights % is measured, remaining includes iron (Fe) and inevitable impurity, has face-centred cubic structure (FCC, Face-Centered Cubic)。
The tissue of the iron-nickel alloy foil is not face-centred cubic structure (FCC), but is formed simultaneously with face-centred cubic structure (FCC) when and body-centered cubic structure (BCC), or there is body-centered cubic structure (BCC), thermal coefficient of expansion can not be effectively reduced, is deposited Be not suitable for use in OLED materials the problem of.
More specifically, the texture coefficient sum in the present invention preferably (111) face and (200) face relative to (111) face, (200) face, (220) face texture coefficient (Texture Coefficient) summation ratio be 80~98%, (111) face The ratio of texture coefficient is 60~78%, and the ratio of the texture coefficient in (200) face is 20~30%, the texture coefficient in (220) face Ratio (include 0%) for less than 20%.
If the size range of the texture coefficient can not be met, generated heat along the width of iron-nickel alloy foil swollen more Swollen difference of coefficients, therefore, the problem of size difference of substrate and mask can occur when process is deposited.
Wherein, texture coefficient (TC) is identified below, i.e. using X-ray diffraction method (XRD), as shown in Fig. 2 obtaining After diffracted intensity peak (Peak) value of each crystal plane, compared with reference peak, changed in the range of by following mathematical expressions 2 Calculate.In following mathematical expressions 2, I (hkl) represents the measure diffracted intensity to (hkl) face, I0(hkl) ASTM (American are represented Society of Testing Materials, American society for testing and materials) standard powder shape diffraction data standard diffraction it is strong Degree.
[mathematical expression 2]
TC(hkl)≥{I(hkl)/I0(hkl)}/[1/n∑{I(hkl)/I0(hkl)}]
The preferred nickel content of iron-nickel alloy foil of the application with texture coefficient as described above is 36~45 weight %.
When nickel content is low, the problem of thermal coefficient of expansion sharply increases be present, it is therefore preferable that the content of the nickel is 36 weights Measure more than %.But its too high levels and during more than 45 weight %, the thermal coefficient of expansion of Alloy Foil is far longer than glass etc., deposits Can not be suitably used as OLED materials the problem of.
Therefore, in the present invention, it is preferred to which the nickel content of iron-nickel alloy foil is limited into 36~45 weight %.
Remaining composition in addition to the nickel content is Fe.But, can be from raw material or surrounding in common manufacturing process Environment is inevitably mixed into unintentional impurity, thus can not be excluded.These impurity are the technologies of usual manufacturing process What personnel both knew about, thus entire contents not specifically mentioned in this manual.
With aforementioned texture and the iron-nickel alloy foil of the application of nickel content is controlled, due to thermal coefficient of expansion Meet 3.0~5.0ppm/K, so as to realize the low thermal coefficient of expansion as target.
In addition, the surface roughness (Rz) of the iron-nickel alloy foil of the present invention is less than 2 μm, satisfaction is used as OLED materials Required condition (JIS specifications), and then, there is the characteristic that the deviation of weight of width and length direction is less than 3%.
Once surface roughness (Rz) is more than 2 μm, then due to surface heterogeneity, during etching work procedure, it is deep to there is generation etching Spend the possibility of difference.
In addition, if the width of Alloy Foil and the deviation of weight of length direction more than 3%, then on surface, generation physical property is inclined Difference, curling increase, thermal coefficient of expansion be present becomes inhomogenous problem.
Wherein, deviation of weight is calculated by following manner, i.e. by iron-nickel alloy foil be cut into 5.8cm × 5cm area and After manufacturing test piece, determine the weight of the test piece, after being converted into the Fe-Ni alloy gravimetric value of unit area, perform repeatedly along iron- The width of nickel alloy foil cuts the process of the test piece, after the iron-nickel alloy foil gravimetric value for determining each test piece, calculates standard Deviation.
As described above, by iron-nickel alloy foil organize the formation of for face-centred cubic structure while, control between face now Ratio, it may thereby be ensured that intensity and ductility are respectively 1.0~1.5GPa, 1~5%.
The iron-nickel alloy foil of the application with the physical property is preferably with 4~50 μm of thickness.
On the other hand, iron-nickel alloy foil of the invention can manufacture according to electrocasting, specifically, contain bag Negative electrode and anode are set in the electrolytic cell of the electrolyte of iron containing compoundses and nickel compound, potential is applied by current device, from And Fe-Ni alloy/C electro-deposition is manufactured in cathode surface.
In the present invention, it is not particularly limited for manufacturing the method for iron-nickel alloy foil with electrocasting, preferably shows as one Example, preferably use nickel, below 20g/L (except 0) that the iron for being 5~20g/L comprising concentration, concentration are 20~50g/L chlorine, The electrolyte of below 5g/L (except 0) boron, below 100ppm (except 0) saccharin.
Boron and saccharin in the bath composition are to obtain conjunction smooth and that glossiness is excellent Goldleaf and the composition added, particularly saccharin, it is to be used to Alloy Foil surface is assigned gloss and obtained trickle The polishing material of film layer, while be also the stress moderator that can alleviate stress.
Wherein, can be with micro addition ascorbic acid for the purpose for preventing electrolyte oxidation.
The remaining solvent of the electrolyte is preferably pure water, it is highly preferred that ultra-pure water can be used.
In addition, the iron that concentration is 5~20g/L can dissolve under the form of the salt such as ferric sulfate, iron chloride, sulfamic acid iron Use, or electrolytic iron, iron powder are dissolved in hydrochloric acid or sulfuric acid and supplied.Moreover, the nickel that the concentration is 20~50g/L can be with The salt form of nickel chloride, nickel sulfate, nickel sulfamic acid etc. uses, or dissolves dilval etc. in acid and supply.
With the Fe-Ni alloy/C paper tinsel of electrocasting manufacture not only because of Fe, Ni concentration inside electrolyte, and can be because in addition The species and content of the composition of addition, process conditions etc. and it is different.If for example, due to the concentration of iron liter inside electrolyte be present The Fe compositions rise of height, then alloy, if current density reduces, the relation such as Fe compositions rise, therefore they are controlled It is critically important.
Particularly in the present invention, iron and nickel concentration and process conditions are manufacture iron-nickel alloy foils during electroforming in electrolyte When obtain needed for texture coefficient important means, the relation of iron ion and nickel ion in particularly described electrolyte is preferably following State the f_Ni of [mathematical expression 1] expression2+Value meets 72~78.
[mathematical expression 1]
f_Ni2+={ [Ni2+]/([Ni2+]+[Fe2+])}×100
(wherein, Ni2+And Fe2+Refer to nickel ion concentration and iron concentration in electrolyte.)
For using the manufacture of the iron-nickel alloy foil of electrocasting, because the nickel that noble metal is used for as the iron of base metal is first The alloy Abnormal Codeposition (anomalous codeposition) of precipitation and show complexity state, even if in order to obtain The composition needed, if it is considered that the ratio between ion dissolved in real solution, then in view of the electrodeposit combination of electro-deposition, Ni ions are dense Degree should be relatively more more than Fe ion concentration.
Therefore, the f_Ni represented with [mathematical expression 1]2+When value meets 72~78, can obtain both has face-centered cubic Structure (FCC) structure has the iron-nickel alloy foil of required nickel content again.
If f_Ni2+It is worth less than 72 or more than 78, then forms the iron-nickel alloy foil with FCC+BCC mixed crystallization structures, The thermal coefficient of expansion of target level can not be ensured.
When using the electrolyte controlled as described above to obtain the iron-nickel alloy foil of the application, preferably with 1.5~ 2.5 pH, 45~70 DEG C of temperature, 10~40A/dm2Current density and 20~45m3/ hr flow condition is implemented.
Now, if pH is too low, when manufacturing iron-nickel alloy foil, can not continuously make because indenture (pit) occurs for surface Industry, nickel composition reduce, and the problem of being difficult to produce the iron-nickel alloy foil of required composition be present.But, if pH is too high, by In electrolyte sludge occurs, the problem of there is also that can not work continuously, nickel composition excessively rises, and required group can not be produced by existing Into iron-nickel alloy foil the problem of.
In view of this point, preferably described pH meets 1.5~2.5.
If current density is too low or too high, the crystalline texture of generation FCC+BCC mixing, the nickel for causing Alloy Foil be present The problem of composition can not meet target level.
It is therefore preferable that the current density is in 10~40A/dm2In the range of set, to form FCC crystalline textures.
In addition, it is too high or in the case that flow is too low even in temperature, also form the crystalline texture of FCC+BCC mixing.
Moreover, there are the following problems, i.e. if temperature is too high or flow is too low, nickel composition reduces, if on the contrary, temperature It is excessive to spend low or flow, then the increase of nickel composition.
It is therefore preferable that the temperature control, at 45~70 DEG C, the flow control is in 20~45m3/ hr, and in the scope It is interior to be set in a manner of forming FCC crystalline textures.
Below by embodiment, the present invention is further illustrated.But it should be noted that following embodiments are served only for pair The present invention is illustrated and embodied, and is not intended to limit the interest field of the present invention.Because the interest field of the present invention By claims record item and thus the item of reasonable analogies determines.
(embodiment)
Containing be 5~20g/L comprising concentration iron, the nickel that concentration is 20~50g/L, below 20g/L chlorine, 5g/L with Under boron, below 100ppm saccharin electrolyte electrolytic cell in, with 1.5~2.5 pH, 45~70 DEG C Temperature, 10~40A/dm2Current density and 20~45m3/ hr flow supplies the electrolyte, has manufactured Fe-Ni alloy Paper tinsel.
The crystalline texture and thermal coefficient of expansion of each iron-nickel alloy foil of manufacture are measured, the results are shown in down State in table 1.Now, crystalline texture is confirmed that texture coefficient is according to aforementioned content by X-ray diffraction analysis Obtain.
In addition, in order to determine mechanical properties, stretching strength determination test piece is made by ASTM-SUB benchmark, by rate of straining (Strain Speed) 1 μm/sec benchmark, are determined using fine cupping machine.
Moreover, metal ion content ratio (f_Ni in measure electrolyte2+) and manufacture iron-nickel alloy foil nickel content, Together it is shown in table 1 below.
【Table 1】
It has been confirmed that the iron-nickel alloy foil for the example 1~12 that the condition of the application is all met and manufactured is respectively provided with FCC configuration, show relatively low thermal coefficient of expansion result.
On the contrary, f_Ni2+Value is unsatisfactory for the comparative example 1~8 of the condition of the application, has been respectively formed FCC and BCC mixed structures, Therefore, thermal coefficient of expansion is high, shows the characteristic for being not suitable for use in OLED materials.
According to nickel content, the thermal coefficient of expansion of the example 1~12 and comparative example 1~8 is shown with chart.
As shown in Fig. 2 it has been confirmed that the thermal coefficient of expansion of the example with FCC configuration is than with FCC+BCC structures Comparative example is low.
Fig. 3 illustrate the present invention iron-nickel alloy foil X-ray diffraction analysis result, can confirm that appearance (111), And (220) peak (200).
In addition, Fig. 4 illustrates the X-ray diffraction analysis result of the iron-nickel alloy foil with FCC-BCC structures, can be true Recognize, not only show the peak of FCC configuration, also together show the peak of BCC structures.

Claims (9)

  1. A kind of 1. iron-nickel alloy foil, it is characterised in that it is the iron-nickel alloy foil manufactured with electrocasting,
    The content of nickel is 36~45 weight %, and remaining includes iron (Fe) and inevitable impurity,
    The Alloy Foil is organized as face-centred cubic structure i.e. FCC, the texture coefficient sum in (111) face and (200) face relative to (111) face, (200) face, (220) face texture coefficient summation ratio be 80~98%, the ratio of the texture coefficient in (111) face Rate is 60~78%, and the ratio of the texture coefficient in (200) face is 20~30%, and the ratio of the texture coefficient in (220) face is 20% Below and include 0%.
  2. 2. iron-nickel alloy foil according to claim 1, wherein, the thermal coefficient of expansion of the iron-nickel alloy foil is that CTE is 3.0~5.0ppm/K.
  3. 3. iron-nickel alloy foil according to claim 1, wherein, the surface roughness of the iron-nickel alloy foil is that Rz is 2 μ Below m.
  4. 4. iron-nickel alloy foil according to claim 1, wherein, the width or length direction of the iron-nickel alloy foil Deviation of weight be less than 3%.
  5. 5. iron-nickel alloy foil according to claim 1, wherein, the tensile strength of the iron-nickel alloy foil for 1.0~ 1.5GPa, extensibility are 1~5%.
  6. 6. iron-nickel alloy foil according to claim 1, wherein, the iron-nickel alloy foil has 4~50 μm of thickness.
  7. 7. a kind of manufacture method of iron-nickel alloy foil, it is characterised in that be to utilize the electrolysis comprising iron compound and nickel compound The method that liquid manufactures iron-nickel alloy foil with electrocasting,
    The relation of iron ion and nickel ion is represented with following mathematical expressions 1 in the electrolyte, the f_Ni of following mathematical expressions 12+Value is full Foot 72~78,
    Mathematical expression 1
    f_Ni2+={ [Ni2+]/([Ni2+]+[Fe2+])}×100
    Wherein, Ni2+And Fe2+Refer to nickel ion concentration and iron concentration in electrolyte.
  8. 8. the manufacture method of iron-nickel alloy foil according to claim 7, wherein, the electrolyte include concentration be 5~ 20g/L iron, concentration are 20~50g/L nickel, below 20g/L chlorine, below 5g/L boron, below 100ppm adjacent sulphonyl benzene Carboximide.
  9. 9. the manufacture method of iron-nickel alloy foil according to claim 7, wherein, Fe-Ni alloy/C is manufactured with the electrocasting During paper tinsel, by 1.5~2.5 pH, 45~70 DEG C of temperature, 10~40A/dm2Current density and 20~45m3/ hr flow enters OK.
CN201710795285.6A 2016-09-08 2017-09-06 Iron-nickel alloy foil and method for producing same Expired - Fee Related CN107805761B (en)

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Cited By (2)

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CN114737132A (en) * 2021-08-10 2022-07-12 山东盛阳金属科技股份有限公司 N06600 iron-nickel base alloy hot continuous rolling plate coil production process
CN115679219A (en) * 2022-11-14 2023-02-03 寰采星科技(宁波)有限公司 Iron-nickel alloy foil for precise metal mask plate and preparation method thereof

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