CN103981484A - Method for quickly fattening solutions on surface of flexible metal strip - Google Patents
Method for quickly fattening solutions on surface of flexible metal strip Download PDFInfo
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Abstract
The invention relates to a method for quickly fattening solutions on the surface of a flexible metal strip, and belongs to the technical field of the preparation of strips of a high temperature superconducting coating conductor. The method provided by the invention comprises the following steps: (1) preparing pioneer liquid 1 using aluminium nitrate, ethanol and yttrium acetate in proportions; (2) preparing pioneer liquid 2 using the yttrium acetate and propanoic acid in proportions; (3) continuously cleaning the metal strips using acetone at a certain speed; (4) continuously cleaning the metal strip using the ethanol at a certain speed; (5) preparing an amorphous yttrium aluminum oxide film using continuous tape feeding and ladder warming equipment to perform coating and heat treatment on the pioneer liquid 1; (6) carrying out coating and heat treatment on the pioneer liquid 2 to prepare an amorphous yttrium oxide film with a smooth surface using the continuous tape feeding and ladder warming equipment. According to the method, continuous tape feeding and ladder warming and annealing are used for increasing the speed of preparing amorphous oxide films, the prepared oxide films not only level the surface of a metal base band, but also stop metal atoms from diffusing towards a superconducting layer at high temperature, and a key technology for preparing the high temperature superconducting strip at a low cost is disclosed.
Description
Technical field
The invention belongs to s-generation belt material of high temperature superconduct technical field, relate to the method for the quick planarization of metal base band surface solution in s-generation belt material of high temperature superconduct.
Background technology
S-generation belt material of high temperature superconduct is one of the study hotspot in high temperature superconducting materia field, and its preparation comprises two portions: the preparation of biaxial texture base band and functional layer preparation.Biaxial texture base band preparation technology can be divided into two large classes: ion beam assisted deposition (Ion Beam Assisted Deposition, be abbreviated as IBAD) and the auxiliary biaxial texture technology (Rolled Assisted Biaxially Textured Substrates, is abbreviated as RABiTS) of rolling.Ion beam assisted deposition (IBAD) does not have particular requirement to the material of metal base band, and Hastelloy and the stainless steel capital can be used as base band material, and ion beam assisted depositing magnesium oxide can obtain needed texture fast.But ion beam assisted depositing magnesium oxide requires the very smooth metal base band in surface, requires surfaceness to be less than 2 nanometers.Polishing metal base band can adopt traditional glossing as mechanical polishing and electrochemical etching.Mechanical polishing process cost is high, efficiency is low, is unsuitable for the surface finish of the long band in flexible metal; Electrochemical etching technique is only applicable to some specific sheet metal strips, and chemical waste fluid is to environment, and treatment cost of waste liquor is higher.
A kind of new ganoid method of metal base band that makes is solution flattening method, it passes through at flexible metal base band surface-coated one deck oxide precursor liquid, utilize surface tension effects, few in raised areas debris, many in trench region debris, liquid film plays leveling effect as continuous integral body to base band surface; Then through Overheating Treatment, forerunner's liquid film volatilizees, resolves into amorphous oxide film.Amorphous oxide film is compared original metal base band, and surface irregularity reduces greatly.By repeatedly repeating above step, surfaceness constantly reduces, and surfaceness can reach below 1 nanometer, can be used as the magnesian base band of ion beam assisted depositing biaxial texture.The amorphous oxide film of preparing by solution flattening method is smooth surface not only, and thickness is adjustable, can also stop the diffusion of metal base band atom under high temperature, prevents that atoms metal from diffusing into superconducting layer and destroying supraconductivity.This method has low cost, is applicable to the feature of large-scale production.But this method also has shortcoming, the thermal treatment of solution flattening method generates in amorphous oxides membrane process, has both had organism volatilization process, also has decomposition course, and for preventing defect, heat-up rate can not be too large, causes tape running speed slower.In order to realize low cost, surface, quick solution planarization flexible metal, adopt continuous tape transport, ladder-elevating temperature is an effective way.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of continuously, fast by flexible metal band uneven surface planarization, can be applied to conductor of high-temperature superconductor coat band and other needs the situation of smooth surface flexible metal base band.
The technical scheme that the present invention solve the technical problem employing is, adopts continuous tape transport, ladder-elevating temperature, and conductor of high-temperature superconductor coat base band solution flattening method, is characterized in that, comprises the steps:
(1) precursor liquid 1 preparation: aluminum nitrate and alcohol solvent are dissolved by predetermined proportion, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add a certain proportion of acetic acid yttrium, be stirred and heated to 50-60 degree and accelerate to dissolve, then add and add again ethanol, make in precursor liquid 1, aluminum ion is 1:1 with the ratio of ruthenium ion concentration, and aluminium ion concentration is 0.1-0.4mol/l.
(2) precursor liquid 2 preparations: acetic acid yttrium and propionic acid are dissolved in proportion, finally add propionic acid solvent, make ruthenium ion concentration 0.05-0.3mol/l in precursor liquid 2.
(3) metal base band acetone cleans: by installing flexible metal band shown in Fig. 1, acetone is poured into shown in Fig. 1 in 3 liquid baths, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 30-50 m/h through three acetone liquid baths.Round work repeatedly.
(4) metal base band ethanol cleans: three liquid baths in step (3) are changed to ethanol, ultrasonic device work, sheet metal strip with the speed order of 30-50 m/h through three ethanol liquid baths.Round work repeatedly, is opened tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 200-250 degree.
(5) apply and thermal treatment precursor liquid 1: with the continuous tape transport zone heating equipment shown in Fig. 1, apply and heat precursor liquid 1, in Fig. 1,6 tube furnace situations are identical, are all divided into A, B, tri-warm areas of C, and the temperature of A is the highest, the temperature of C is minimum, and the temperature difference of adjacent warm area can be set 10-40 degree.Shown in Fig. 1, in 3 liquid baths, containing precursor liquid 1, open tube furnace 2,4,6, the temperature difference of three warm areas equates, for 10-20 degree, setting C district temperature is 560-600 degree, and sheet metal strip passes through liquid bath with the speed of 40-100 m/h, then heating, often walk once, on metal base band, applied three layers of yttrium alumite.Repeatedly, can obtain the amorphous yttrium alumite of different thickness.
(6) apply also thermal treatment precursor liquid 2: the precursor liquid in step (5) is changed to precursor liquid 2, the temperature difference of three warm areas equates, for 10-20 degree, setting C district temperature is 500-580 degree, sheet metal strip passes through liquid bath with the speed of 60-150 m/h, then heating, often walks once, has applied three layers of yttrium oxide film on metal base band.Repeatedly, can obtain the amorphous yttrium oxide film of different thickness, until obtain film surface r.m.s. roughness, in 5 * 5 square microns, be less than 2 nanometers.
(7), in described step (3) (4) (5) (6), metal base band is Hastelloy base band or stainless steel base band, in untreated front surface 5 * 5 square microns, and r.m.s. roughness 20-60 nanometer.
(8), in described step (6) (7), surperficial r.m.s. roughness adopts atomic force microscope test to obtain.
Accompanying drawing explanation
For technical scheme of the present invention and embodiment are clearly described, will the accompanying drawing of required use in invention technical description and embodiment be briefly introduced below.
Fig. 1 is continuous tape transport, ladder-elevating temperature equipment schematic diagram.
Fig. 2 is the X-ray diffraction θ-2 θ scintigram of embodiment mono-.
Fig. 3 is atomic force microscope (AFM) figure of embodiment mono-.
Embodiment
Embodiment mono-: on Hastelloy 276 chemical solution method prepare fast AlYO Y
2o
3noncrystal membrane, for the method for conductor of high-temperature superconductor coat base band planarization, comprises the steps:
(1) precursor liquid 1 preparation: get 67.5 grams of aluminum nitrates and 1500 milliliters of dissolve with ethanol, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add 61 grams of acetic acid yttriums, being stirred and heated to 50 degree accelerates to dissolve, then add and add ethanol to make volume reach 1800 milliliters again, making aluminium ion concentration in precursor liquid 1 is 0.1mol/l.
(2) precursor liquid 2 preparations: 60.8 grams of acetic acid yttriums are pressed and dissolved with 1600 milliliters of propionic acid, finally add propionic acid to make volume reach 1800 milliliters, making ruthenium ion concentration in precursor liquid 2 is 0.1mol/l.
(3) metal base band acetone cleans: by installing flexible metal band shown in Fig. 1,1800 milliliters of acetone are poured into respectively shown in Fig. 1 in 3 liquid baths, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 30 ms/h through three acetone liquid baths.The work of coming and going 3 times.
(4) metal base band ethanol cleans: three liquid baths in step (3) are changed to ethanol, ultrasonic device work, sheet metal strip with the speed order of 30 ms/h through three ethanol liquid baths.The work of coming and going 3 times, opens tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 230 degree.
(5) apply also thermal treatment precursor liquid 1: in 3 liquid baths shown in Fig. 1, contain respectively 600 milliliters of precursor liquids 1, the temperature difference of first opening 2,4,6, three warm areas of tube furnace equates, be 10 degree, setting C district temperature is 570 degree, and sheet metal strip passes through liquid bath with the speed of 50 ms/h, then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, the temperature difference of three warm areas equates, is 10 degree, and setting C district temperature is 570 degree, sheet metal strip with the speed of 50 ms/h through liquid bath, then heating.Repeat 2 times like this, surfaceness is 2.2 nanometers.
(6) apply also thermal treatment precursor liquid 2: the precursor liquid in step (5) is changed to the precursor liquid 2 that ruthenium ion concentration is 0.1mol/l, and setting C district temperature is 510 degree, and the temperature difference of three warm areas equates, be 10 degree, sheet metal strip is walked to the right with the speed of 60 ms/h, through liquid bath, and then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, setting C district temperature is 510 degree, and the temperature difference of three warm areas equates, is 10 degree, and sheet metal strip is walked left with the speed of 60 ms/h.Repeat 2 times, XRD test result as shown in Figure 2, shows that film is non-crystal structure, and surfaceness is 1.2 nanometers, as shown in Figure 3.
Embodiment bis-: on Hastelloy 276 chemical solution method prepare fast AlYO Y
2o
3noncrystal membrane, for the method for conductor of high-temperature superconductor coat base band planarization, comprises the steps:
(1) precursor liquid 1 preparation: get 135 grams of aluminum nitrates and 1700 milliliters of dissolve with ethanol, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add 122 grams of acetic acid yttriums, being stirred and heated to 60 degree accelerates to dissolve, then add and add ethanol to make volume reach 1800 milliliters again, making aluminium ion concentration in precursor liquid 1 is 0.2mol/l.
(2) precursor liquid 2 preparations: 30.4 grams of acetic acid yttriums are pressed and dissolved with 1700 milliliters of propionic acid, finally add propionic acid to make volume reach 1800 milliliters, making ruthenium ion concentration in precursor liquid 2 is 0.05mol/l.
(3) metal base band acetone cleans: by installing flexible metal band shown in Fig. 1,1800 milliliters of acetone are poured into respectively shown in Fig. 1 in 3 liquid baths, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 40 ms/h through three acetone liquid baths.The work of coming and going 3 times.
(4) metal base band ethanol cleans: three liquid baths in step (3) are changed to ethanol, ultrasonic device work, sheet metal strip with the speed order of 50 ms/h through three ethanol liquid baths.The work of coming and going 3 times, opens tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 250 degree.
(5) apply also thermal treatment precursor liquid 1: in 3 liquid baths shown in Fig. 1, contain respectively 600 milliliters of precursor liquids 1, the temperature difference of first opening 2,4,6, three warm areas of tube furnace equates, be 15 degree, setting C district temperature is 590 degree, and sheet metal strip passes through liquid bath with the speed of 70 ms/h, then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, the temperature difference of three warm areas equates, is 10 degree, and setting C district temperature is 590 degree, sheet metal strip with the speed of 70 ms/h through liquid bath, then heating.Repeat 2 times like this, surfaceness is 1.9 nanometers.
(6) apply also thermal treatment precursor liquid 2: the precursor liquid in step (5) is changed to the precursor liquid 2 that ruthenium ion concentration is 0.05mol/l, and setting C district temperature is 530 degree, and the temperature difference of three warm areas equates, be 10 degree, sheet metal strip is walked to the right with the speed of 80 ms/h, through liquid bath, and then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, setting C district temperature is 530 degree, and the temperature difference of three warm areas equates, is 10 degree, and sheet metal strip is walked left with the speed of 80 ms/h.Repeat 2 times, surfaceness is 0.9 nanometer.
Claims (9)
1. the quick solution flattening method of flexible metal strip surface, is characterized in that, comprises the following steps:
(1) precursor liquid 1 preparation: aluminum nitrate and alcohol solvent are dissolved by predetermined proportion, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add a certain proportion of acetic acid yttrium, be stirred and heated to 50-60 degree and accelerate to dissolve, then add and add again ethanol, make in precursor liquid 1, aluminum ion is 1:1 with the ratio of ruthenium ion concentration, and aluminium ion concentration is 0.1-0.4mol/l;
(2) precursor liquid 2 preparations: acetic acid yttrium and propionic acid are dissolved in proportion, finally add propionic acid solvent, make ruthenium ion concentration 0.05-0.3mol/l in precursor liquid 2;
(3) metal base band acetone cleans: acetone is poured in the liquid bath of continuous tape transport, ladder-elevating temperature equipment, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 30-50 m/h through three acetone liquid baths; Round work repeatedly;
(4) metal base band ethanol cleans: ethanol is poured in the liquid bath of continuous tape transport, ladder-elevating temperature equipment, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, sheet metal strip with the speed order of 30-50 m/h through three ethanol liquid baths; Round work repeatedly, is opened tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 200-250 degree;
(5) apply also thermal treatment precursor liquid 1: precursor liquid 1 is poured in the liquid bath of continuous tape transport, ladder-elevating temperature equipment; The temperature difference of opening 2,4,6, three warm areas of tube furnace is 10-20 degree, and setting C district temperature is 560-600 degree, and sheet metal strip through three liquid baths, has applied three layers of yttrium alumite with the speed of 40-100 m/h on metal base band; Repeatedly, can obtain the amorphous yttrium alumite of different thickness;
(6) apply also thermal treatment precursor liquid 2: precursor liquid 1 is poured in the liquid bath of continuous tape transport, ladder-elevating temperature equipment; The temperature difference of opening 2,4,6, three warm areas of tube furnace is 10-20 degree, and setting C district temperature is 500-580 degree, and sheet metal strip through three liquid baths, has applied three layers of yttrium oxide film with the speed of 60-150 m/h on metal base band; Repeatedly, can obtain the amorphous yttrium oxide film of different thickness, until obtain film surface r.m.s. roughness, in 5 * 5 square microns, be less than 2 nanometers.
2. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, it is characterized in that, in described step (3) (4) (5) (6), metal base band is Hastelloy base band or stainless steel base band, in untreated front surface 5 * 5 square microns, r.m.s. roughness 20-60 nanometer.
3. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, it is characterized in that, in described step (3) (4) (5) (6), tape transport, ladder-elevating temperature equipment are that metal base band passes through continuously the heating zone of three differing tempss in heat-processed continuously, between adjacent heating zone, temperature difference regulation range is 10-40 degree, and tape running speed regulation range is 30-200 m/h.
4. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, is characterized in that, in described step (1), in precursor liquid 1, aluminum ion is 1:1 with the ratio of ruthenium ion concentration, and aluminium ion concentration scope is 0.1-0.4mol/l.
5. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, is characterized in that, in described step (2), in precursor liquid 2, ruthenium ion concentration range is 0.05-0.3mol/l.
6. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, is characterized in that, in described step (3), sheet metal strip with the speed order of 30-50 m/h through three acetone liquid baths.
7. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, it is characterized in that, in described step (4), sheet metal strip is with the speed order of 30-50 m/h through three ethanol liquid baths, and last tape transport is all set as 200-250 degree tube furnace temperature.
8. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, it is characterized in that, in described step (5), C district temperature setting is set to 560-600 degree, the temperature difference of three warm areas is 10-20 degree, sheet metal strip with the speed of 40-100 m/h through three liquid baths.
9. the quick solution flattening method of a kind of flexible metal as claimed in claim 1 strip surface, it is characterized in that, in described step (6), C district Temperature Setting is 500-580 degree, the temperature difference of three warm areas is 10-20 degree, sheet metal strip with the speed of 60-150 m/h through three liquid baths
.
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