CN101307429A - Process for preparing high-purity metallic nickel target of superfine crystal particle - Google Patents
Process for preparing high-purity metallic nickel target of superfine crystal particle Download PDFInfo
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- CN101307429A CN101307429A CNA2008100317497A CN200810031749A CN101307429A CN 101307429 A CN101307429 A CN 101307429A CN A2008100317497 A CNA2008100317497 A CN A2008100317497A CN 200810031749 A CN200810031749 A CN 200810031749A CN 101307429 A CN101307429 A CN 101307429A
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Abstract
The invention relates to a method for preparing metallic nickel target materials with superfine crystal grains and high purity. The method comprises the following steps of vacuum melting, rolling processing and heat treatment, wherein, the step of vacuum melting and purification mainly guarantees the high purity of nickel targets, and the step of rolling processing and the step of heat treatment mainly aim to guarantee the fineness of the crystal grains of the nickel targets. The grain diameter of the metallic nickel target materials prepared by adoption of the method is fine and is between 20 and 30 micrometers, which is far lower than 100 micrometers required; the purity of the metallic nickel target materials is high and reaches over 99.9 percent; and the metallic nickel targets have uniform structural constituents and can be mechanically processed into high-quality high-purity metallic nickel targets subsequently.
Description
Technical field
The present invention relates to the high-purity metallic nickel target of superfine crystal particle that a kind of vacuum splashing and plating is used, belong to metallic substance, vacuum surface Coating Materials, metallic substance press working and thermal treatment field.
Background technology
In recent years, along with the enhancing of people to environmental protection and energy dilemma consciousness, the surface coating technology of material carries out the transition to the vacuum splashing and plating technology gradually by traditional plating and electroless plating technology.Vacuum magnetic control sputter technology has obtained using widely at five metals decoration and protective coating, electronic product coating, electromagnetic shielding plated film, plastics plated film and automobile and building glass plated film field.Therefore, the sputtering target material demand that will use as this technology plated film rete also just seems more urgent.
Nickel has obtained to use widely as a kind of most typical vacuum splashing and plating metallic substance.Because the corrosion resistance of nickel is good, capability of electromagnetic shielding is good, and can be used as important characteristic such as energy and material use, adopts vacuum splashing and plating nickel to become the important production field that surface coating is handled.Nickel can decorate as five metals in other metallic surfaces and protective coating uses.The most important starting material sponge nickel that uses in nickel metal hydride battery also can be produced by the mode of nickel target vacuum splashing and plating.The compliant conductive cloth surface of using in electromagnetic shielding material also uses the nickel target as the sputter source.In addition, all used the nickel target in a large number in fields such as plastics metal-coated membrane, building glass metal-coated membranes.
The processing of target has strict requirement to many-sides such as material and facilities, but the material that uses at target itself, key must reach service requirements in the performance aspect 3: (1) material purity height.At least in 99.9% above purity, other all impurity elements in the target are all needed strict control and detection, guarantee the guarantee of the smooth implementation and the coating performance of vacuum sputtering process; (2) crystal grain is tiny.The grain-size of high quality target requirement at present all below 100 μ m, could improve the homogeneity of vacuum-coating like this, reaches the requirement of functions of use index, especially can improve the utilization ratio of target, improves the production efficiency of vacuum splashing and plating; (3) machining accuracy height.For various circles, rectangle, tubular target, strict size tolerance requirements is all arranged, satisfy the requirement of production process assembling.And in above-mentioned requirements, require highly purified metallic substance to possess tiny and uniform crystal grain simultaneously, and be to be difficult to satisfied simultaneously index, the pure metal material purity is high more, the difficult more control of inner grain-size, crystal grain is easy more grows up.Therefore, exploitation superfine crystal particle high purity metal target becomes the problem of an important target material exploitation.
The processing of nickel target is difficult to satisfy the condition that target uses, and main shortcoming is that the purity of nickel material is low, and especially grain-size is thick.Generally about 99.8%, foreign matter content is the content height of Fe, C especially for anode nickel plates material purity after the electrolysis of present domestic process, causes the sputtered layer pollution and blackspot occurs.In addition, a large amount of metallic nickel targets of present domestic use are not controlled grain-size, grain-size is excessive, seriously exceed the target requirement 100 μ m the index several times in addition surpass an order of magnitude, such nickel target can't satisfy the service requirements of high quality sputtered layer.
Summary of the invention
The present invention is directed to high purity (more than 99.9%) and close grain (less than 100 μ m) requirement that target uses, a kind of method for preparing high-purity metallic nickel target of superfine crystal particle is provided, adopt this method to obtain purity more than 99.9%, grain-size is at the high-test metal nickel target of 20～30 μ m.
A kind of method for preparing high-purity metallic nickel target of superfine crystal particle, comprise starting material are carried out vacuum melting, rolling processing and thermal treatment, wherein to purify mainly be the high purity that guarantees the nickel target in vacuum melting, rolling processing and thermal treatment be for the crystal grain that guarantees the nickel target tiny.
Starting material sheet nickel purity is directly carried out surface finish more than 99.9%, removes surface scale;
Starting material sheet nickel purity is lower than 99.9%, then the starting material anode nickel plates is carried out melting and casting in vacuum oven, and vacuum tightness reaches 6 * 10
-1Below the MPa, 1500 ℃～1700 ℃ of smelting temperatures directly are cast as the nickel ingot in the water-cooled swage under the vacuum condition;
The nickel ingot is carried out the surface plane mill, the defective of nickel ingot surface is milled remove; To carry out cold rolling under the room temperature through the nickel ingot of surperficial milling, rolling reduction surpasses more than 50%, guarantees that enough deflections realize the abundant fragmentation of nickel ingot interior tissue and evenly.
Nickel plate after cold rolling at 600 ℃～800 ℃ following annealing 30min～120min, is carried out then taking out from stove and carries out water-cooled or the air apoplexy is blown cool to room temperature, obtain the nickel target blank that needs.
This blank is carried out mechanical workout, obtain the high-purity superfine crystal grain nickel target that needs.
The grain-size of the metallic nickel target that employing the present invention makes is tiny, at 20～30 μ m, far below the grain-size of the 100 μ m that require; The purity height of metallic nickel target reaches more than 99.97%; Metallic nickel target tissue composition is even, can follow-uply be machined into high-quality high-purity metal nickel target.
Description of drawings
Fig. 1: superfine crystal particle nickel target grain-size microstructure;
Fig. 2: through the Ni target outward appearance photo of mechanical workout.
Embodiment
Embodiment 1:
More than 99.9%, carry out surface finish at starting material sheet nickel purity, scale removal presents metalluster, directly cut out to be rolled.
Carry out cold rolling under the room temperature through the slab ingot of surperficial milling, rolling reduction surpasses more than 50%, guarantees that enough deflections realize the abundant fragmentation of nickel ingot interior tissue and evenly.
Nickel plate after cold rolling at 600 ℃ of 30min that anneal down, is carried out then taking out from stove and carries out water-cooled, obtain the nickel target blank that needs.This blank is carried out mechanical workout, and the size that acquisition needs then obtains the high-purity superfine crystal grain nickel target that needs.
The nickel target purity that obtains is 99.96%, average grain size 24 μ m.
Embodiment 2:
More than 99.9%, carry out surface finish at starting material sheet nickel purity, scale removal presents metalluster, directly cut out to be rolled.
Carry out cold rolling under the room temperature through the slab ingot of surperficial milling, rolling reduction surpasses more than 50%, guarantees that enough deflections realize the abundant fragmentation of nickel ingot interior tissue and evenly.
Nickel plate after cold rolling at 700 ℃ of 60min that anneal down, is carried out taking out from stove then, blow cool to room temperature, obtain the nickel target blank that needs in the air apoplexy.This blank is carried out mechanical workout, and the size that acquisition needs then obtains the high-purity superfine crystal grain nickel target that needs.
The nickel target purity that obtains is 99.95%, average grain size 27 μ m.
Embodiment 3:
More than 99.9%, carry out surface finish at starting material sheet nickel purity, scale removal presents metalluster, directly cut out to be rolled.
Carry out cold rolling under the room temperature through the slab ingot of surperficial milling, rolling reduction surpasses more than 50%, guarantees that enough deflections realize the abundant fragmentation of nickel ingot interior tissue and evenly.
Nickel plate after cold rolling at 800 ℃ of 120min that anneal down, is carried out then taking out from stove and carries out water-cooled, obtain the nickel target blank that needs.This blank is carried out mechanical workout, and the size that acquisition needs then obtains the high-purity superfine crystal grain nickel target that needs.
The nickel target purity that obtains is 99.97%, average grain size 29 μ m.
Embodiment 4:
Starting material sheet nickel purity is lower than 99.9%, then the starting material anode nickel plates is carried out melting and casting in vacuum oven, and vacuum tightness reaches 10
-2Below the MPa, 1700 ℃ of smelting temperatures, vacuum condition directly are cast as the slab ingot that needs down in the water-cooled swage.
Carry out cold rolling under the room temperature through the slab ingot of surperficial milling, rolling reduction surpasses more than 50%, guarantees that enough deflections realize the abundant fragmentation of nickel ingot interior tissue and evenly.
Nickel plate after cold rolling at 800 ℃ of 120min that anneal down, is carried out then taking out from stove and carries out water-cooled, obtain the nickel target blank that needs.This blank is carried out mechanical workout, and the size that acquisition needs then obtains the high-purity superfine crystal grain nickel target that needs.The nickel target purity that obtains is 99.92%, grain-size 28 μ m.
Claims (2)
1. method for preparing high-purity metallic nickel target of superfine crystal particle, it is characterized in that: comprise starting material are carried out vacuum melting, rolling processing and thermal treatment, specific embodiment is:
Purity is lower than 99.9% starting material anode nickel plates and carries out melting and casting in vacuum oven, vacuum tightness reaches 6 * 10
-1Below the MPa, 1500 ℃～1700 ℃ of smelting temperatures directly are cast as the nickel ingot in the water-cooled swage under the vacuum condition;
The nickel ingot at room temperature carries out cold rolling after the surface plane mills, and rolling reduction is more than 50%;
At 600 ℃～800 ℃ 30min～120min that anneal down, water-cooled or air apoplexy are blown cool to room temperature, obtain the nickel target blank that needs with the nickel plate after cold rolling;
Blank is carried out mechanical workout, then obtain the high-purity superfine crystal grain nickel target that needs;
Described high purity is meant purity more than 99.9%, and described close grain refers to that granularity is less than 100 μ m.
2. method for preparing high-purity metallic nickel target of superfine crystal particle, it is characterized in that: comprise rolling processing and thermal treatment, specific embodiment is:
Purity dug through the surface in the starting material anode nickel plates more than 99.9% at room temperature carry out after milling cold rollingly, rolling reduction is more than 50%;
At 600 ℃～800 ℃ 30min～120min that anneal down, water-cooled or air apoplexy are blown cool to room temperature, obtain the nickel target blank that needs with the nickel plate after cold rolling;
Blank is carried out mechanical workout, then obtain the high-purity superfine crystal grain nickel target that needs;
Described close grain refers to that grain-size is less than 100 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100317497A CN101307429A (en) | 2008-07-14 | 2008-07-14 | Process for preparing high-purity metallic nickel target of superfine crystal particle |
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| CNA2008100317497A CN101307429A (en) | 2008-07-14 | 2008-07-14 | Process for preparing high-purity metallic nickel target of superfine crystal particle |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286666A (en) * | 2011-07-06 | 2011-12-21 | 江苏远航精密合金科技有限公司 | Process for preparing high-weight nickel ingots by vacuum melting method |
| CN109082637A (en) * | 2018-08-15 | 2018-12-25 | 四川省有色冶金研究院有限公司 | A kind of high uniformly fine grain tin target and preparation method thereof of high-purity |
| CN112725675A (en) * | 2020-12-23 | 2021-04-30 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN114000073A (en) * | 2021-10-28 | 2022-02-01 | 宁波江丰电子材料股份有限公司 | Process method for improving internal structure of high-purity nickel target material |
| CN115341185A (en) * | 2022-10-18 | 2022-11-15 | 江苏集萃先进金属材料研究所有限公司 | Target material and manufacturing method thereof |
| CN115449767A (en) * | 2022-09-28 | 2022-12-09 | 昆明理工大学 | Preparation method of fine-grain high-purity nickel target material |
-
2008
- 2008-07-14 CN CNA2008100317497A patent/CN101307429A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286666A (en) * | 2011-07-06 | 2011-12-21 | 江苏远航精密合金科技有限公司 | Process for preparing high-weight nickel ingots by vacuum melting method |
| CN102286666B (en) * | 2011-07-06 | 2013-03-13 | 江苏远航精密合金科技股份有限公司 | Process for preparing high-weight nickel ingots by vacuum melting method |
| CN109082637A (en) * | 2018-08-15 | 2018-12-25 | 四川省有色冶金研究院有限公司 | A kind of high uniformly fine grain tin target and preparation method thereof of high-purity |
| CN112725675A (en) * | 2020-12-23 | 2021-04-30 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN112725675B (en) * | 2020-12-23 | 2021-11-09 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN114000073A (en) * | 2021-10-28 | 2022-02-01 | 宁波江丰电子材料股份有限公司 | Process method for improving internal structure of high-purity nickel target material |
| CN115449767A (en) * | 2022-09-28 | 2022-12-09 | 昆明理工大学 | Preparation method of fine-grain high-purity nickel target material |
| CN115341185A (en) * | 2022-10-18 | 2022-11-15 | 江苏集萃先进金属材料研究所有限公司 | Target material and manufacturing method thereof |
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Open date: 20081119 |