CN104174851A - Preparation method of Co-Cr-Pt-SiO2 target material - Google Patents
Preparation method of Co-Cr-Pt-SiO2 target material Download PDFInfo
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- CN104174851A CN104174851A CN201410394572.2A CN201410394572A CN104174851A CN 104174851 A CN104174851 A CN 104174851A CN 201410394572 A CN201410394572 A CN 201410394572A CN 104174851 A CN104174851 A CN 104174851A
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Abstract
The invention discloses a preparation method of a Co-Cr-Pt-SiO2 target material. The method comprises the steps of selecting raw material powder, mixing the raw material powder, pre-pressing and forming ingot blanks, performing reactive synthesis and sintering procedure, carrying out hot isostatic pressing procedure and finally performing mechanical processing. According to the preparation method, combination of phases in the Co-Cr-Pt-SiO2 target material is effectively improved and enhanced with the adoption of the reaction synthesis sintering technology, the density of the material is improved, performing canning, evacuating, seal welding prior to the conventional hot isostatic pressing and performing decanning processing technology prior to the hot isostatic pressing are avoided, the production technology is effectively simplified, the processing performance of the material is improved, the continuous industrial production is feasible.
Description
Technical field
The invention provides a kind of preparation method of Co base alloy target material, specifically, is a kind of Co-Cr-Pt-SiO for magnetic recording media industry
2preparation of target materials method, belongs to powder metallurgical technology.
Background technology
Target is a kind of extraordinary electronic material with high additive value, at semiconductor microelectronics integrated circuit, thin film hybrid IC, chip components and parts, the technical field such as hard disk, CD and liquid crystal flat panel display LCD particularly, all need by sputtering technology and adopt different preparation of target materials to go out the film of various unlike materials, reaching the performance requirement such as magnetic, electrical, optical, piezoelectricity of product.Target, as the basic technology of sophisticated industry development, has obtained developing on an unprecedented scale, target market scale expanding day specialized rising industry of flourish one-tenth.At present, magnetic recording media target is one of three class targets of market scale maximum.
Along with the continuous growth of magnetic recording density, corresponding magnetic recording media becomes and becomes increasingly complex by the structural component of target, from initial binary Co-Cr alloy, ternary Co-Cr-Pt alloy, Co-Cr-Pt-B to five yuan of Co-Cr-Pt-B-Cu of quaternary.People find gradually with Co-Cr-Pt-SiO in recent years
2for the Co-Cr-Pt-oxide target material representing has excellent magnetic performance, in magnetic recording media industry, be widely used.Due to the existence of oxide, Co-Cr-Pt-SiO
2target is difficult to by conventional melting and plastic working legal system standby, and normally adopts powder metallurgic method to be prepared.For example, U.S. Patent Publication No. US2007/0134124A1, open day on June 14th, 2007, the name of innovation and creation is called Sputter target and method for fabricating sputter target including a plurality of materials, this application case discloses a kind of multicomponent sputtering target material and preparation method thereof, the method by raw material select, powder mixes, compacting, dress jacket, high temperature insostatic pressing (HIP) and machined have obtained Co-Cr-Pt-SiO
2etc. multicomponent target, the method requires to select powder size between 0.01～50 micron, with the splash phenomena that prevents that target from occurring in sputter procedure.Its weak point be before hip treatment, must fill jacket to powder, vacuumize, soldering and sealing; After high temperature insostatic pressing (HIP), need jacket treatment process, technique relative complex, time-consuming length, and in going the process of jacket, easily cause the loss of precious metals pt.
China Patent Publication No. CN101928851A, open day on December 29th, 2010, the name of innovation and creation is called boracic target material and preparation method thereof, film, magnetic recording medium, this application case discloses a kind of preparation method of boracic target material, the method is by preparation Co-Cr prealloy powder, subsequently prealloy powder mixed with boron powder and oxide, sieve, pre-molding, vacuum heating-press sintering prepare Co-Cr-B-oxide target material and Co-Cr-Pt-B-oxide target material, applicant thinks and adopts Co-Cr prealloy powder effectively to avoid the generation of thick boride.Its weak point is, in mixing, having adopted afterwards the processing of sieving is equally also also to avoid one of reason of thick boride generation, due to initial powder granularity and crushing efficiency difference, likely cause composition and predeterminated target composition after sieving to have different simultaneously.
We also find at experimentation simultaneously, and powder metallurgic method is prepared Co-Cr-Pt-SiO
2in the process of target, as adopt directly mixed powder and pressing process moulding, conventionally can run into oxide and be combined the problems such as bad, non-wetting with other composition, cause thus the target defect of preparation more, density is lower, and machining and processability are poor.After retrieval amount of literature data, so far there are no reactive synthesis technique, be applied to prepare Co-Cr-Pt-SiO
2the relevant report of target.This project is applied to Co-Cr-Pt-SiO by reactive synthesis technique
2in the preparation of target, effectively improve combination between each thing phase in composite, thereby the density of material and processing characteristics are all improved significantly.
Summary of the invention
The object of the present invention is to provide a kind of new preparation of target materials method, prepare the Co-Cr-Pt-SiO that oxide particle and metallic matrix have good metallurgical binding
2target.Its preparation process follows these steps to carry out:
(1) carry out the selection of material powder: material powder is Co, Cr, Pt, Si and oxide (Co
3o
4, CoO, Co
2o
3, Cr
2o
3in one or more mixture), purity is all more than or equal to 99.95wt%, Co, Cr, Pt, Si powder size are 1～50 μ m, CoO, Co
3o
4, Co
2o
3, Cr
2o
3granularity is 1～10 μ m;
(2) Co, Cr, Pt, Si and oxide are mixed, wherein the content of Co is 45～65at%, and the content of Cr is 12～35at%, and the content of Pt is 3～20at%, and the content of Si is 4～15at%, and the content of oxide is 2～20at%.Adopt planetary ball mill mode to mix powder, employing medium ball is steel ball, agate ball or zirconia ball, and ratio of grinding media to material is 5:1～20:1, and the mixed powder time is 12～36 hours;
(3) after mixed powder, adopting hydraulic press to carry out pre-molding, is under 10～200MPa, to carry out the pre-molding of 0.5～2 hour at pressure;
(4) the target ingot blank of handling well in step (3) is evacuated to 1x10
-2～1x10
-3pa, then fill Ar gas to 1～20Pa, at 850～1000 ℃, to carry out solid phase reaction and synthesize, the time is 1～4 hour;
(5) the target ingot blank of (4) being handled well carries out hip treatment, and hip temperature is 1000～1500 ℃, and pressure is 100～150MPa, and the time is 1～16 hour;
(6) carry out the target product that mechanical process obtains needing size.
Advantage of the present invention is that the reaction synthesis technique first adopting in the present invention makes SiO
2in sintering process, reaction is synthesized, SiO
2particle is tiny, be evenly distributed, SiO
2be combined well with metallic matrix interface; Secondly before high temperature insostatic pressing (HIP), added single step reaction synthesis technique, effectively improve the target ingot blank density before high temperature insostatic pressing (HIP), avoided must filling jacket to powder before traditional hip treatment, vacuumized, removed jacket treatment process after soldering and sealing and high temperature insostatic pressing (HIP), effectively simplified production technology, eliminated and gone the noble metal loss that causes in jacket process, also improved the processing characteristics of target simultaneously.This method can be widely used in the preparation of metal-oxide composite, is applicable to carrying out successional suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is Co, Cr, Pt, Co
3o
4, the X ray diffracting spectrum after the mixed powder of Si ball milling,
Fig. 2 is for reacting X ray diffracting spectrum (employing Co, Cr, Pt, the Co after synthetic and high temperature insostatic pressing (HIP)
3o
4, Si powder carries out the mixed powder of ball milling),
Fig. 3 for the SEM photo of reaction after synthetic (Fig. 3 a) and corresponding EDS power spectrum (Fig. 3 b) (adopt Co, Cr, Pt, Co
3o
4, Si powder carries out the mixed powder of ball milling).
The specific embodiment
In conjunction with Fig. 1～3 pair the specific embodiment of the present invention, be further described.
Embodiment 1
The material powder of selecting is Co, Cr, Pt, Co
3o
4, five kinds of powder of Si, wherein the content of Co is 50at%, the content of Cr is 28at%, the content of Pt is 16at%, the content of Si is 4at%, Co
3o
4content be 2at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is steel ball, and ratio of grinding media to material is 5:1, and the mixed powder time is 14 hours (Fig. 1 is shown in by the XRD collection of illustrative plates after mixed powder); Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 120MPa, and the dwell time is 0.5 hour, forms target ingot blank; Be evacuated to subsequently 1x10
-3pa, then fill Ar gas to 5Pa, at 900 ℃, to carry out solid phase reaction and synthesize, the time is 2 hours, after processing, the density of target ingot blank is 9.35g/cm
3, reach solid density 95.3% (Fig. 2 is shown in by the XRD collection of illustrative plates after reaction is synthetic, and the SEM after reaction is synthetic is shown in Fig. 3 a), and the EDAX results of black particle 1 in Fig. 3 a (Fig. 3 b) shows that black particle is SiO
2particle, SiO
2particle size distribution scope is 200～1000nm, and average grain diameter is 450nm; The target of handling well is carried out to hip treatment, and hip temperature is 1000 ℃, and pressure is 120MPa, and the time is 2 hours, and after processing, the density of target ingot blank is 9.72g/cm
3, reach 99.1% (Fig. 2 is shown in by the XRD collection of illustrative plates after high temperature insostatic pressing (HIP)) of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-27Cr-15Pt-4SiO
2(at%).
Embodiment 2
The material powder of selecting is Co, Cr, Pt, CoO, five kinds of powder of Si, and wherein the content of Co is 50at%, and the content of Cr is 28at%, and the content of Pt is 10at%, and the content of Si is 4at%, and the content of CoO is 8at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is zirconia ball, and ratio of grinding media to material is 8:1, and the mixed powder time is 24 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 150MPa, and the dwell time is 0.5 hour, forms target ingot blank; Be evacuated to subsequently 5x10
-3pa, then fill Ar gas to 10Pa, at 900 ℃, to carry out solid phase reaction and synthesize, the time is 2 hours, after processing, the density of target ingot blank is 8.66g/cm
3, reach 96.3% of solid density, SiO
2particle size distribution scope is 200～850nm, and average grain diameter is 325nm; The target of handling well is carried out to hip treatment, and hip temperature is 1000 ℃, and pressure is 120MPa, and the time is 2 hours, and after processing, the density of target ingot blank is 8.93g/cm
3, reach solid density solid density 99.3%; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-28Cr-10Pt-4SiO
2(at%).
Embodiment 3
The material powder of selecting is Co, Cr, Pt, Co
2o
3, five kinds of powder of Si, wherein the content of Co is 58at%, the content of Cr is 20at%, the content of Pt is 12at%, the content of Si is 6at%, Co
2o
3content be 4at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is agate ball, and ratio of grinding media to material is 10:1, and the mixed powder time is 18 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, mold pressing pressure is 90MPa, and the dwell time is 1 hour, forms target ingot blank; Be evacuated to subsequently 2x10
-3pa, then fill Ar gas to 15Pa, at 1000 ℃, to carry out solid phase reaction and synthesize, the time is 2.5 hours, after processing, the density of target ingot blank is 8.62g/cm
3, be 96.5% of solid density, SiO
2particle size distribution scope is 400～1000nm, and average grain diameter is 520nm; The target of handling well is carried out to hip treatment, and hip temperature is 1100 ℃, and pressure is 110MPa, and the time is 2.5 hours, and after processing, the density of target ingot blank is 8.88g/cm
3for 99.4% of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-19Cr-12Pt-6SiO
2(at%).
Embodiment 4
The material powder of selecting is Co, Cr, Pt, Cr
2o
3, five kinds of powder of Si, wherein the content of Co is 48at%, the content of Cr is 20at%, the content of Pt is 12at%, the content of Si is 12at%, Cr
2o
3content be 8at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is steel ball, and ratio of grinding media to material is 12:1, and the mixed powder time is 24 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 200MPa, and the dwell time is 1 hour, forms target ingot blank; Be evacuated to subsequently 1x10-
2pa, then fill Ar gas to 18Pa, at 980 ℃, to carry out solid phase reaction and synthesize, the time is 2.5 hours, after processing, the density of target ingot blank is 7.38g/cm
3, be 96.5% of solid density, SiO
2particle size distribution scope is 100～750nm, and average grain diameter is 275nm; The target of handling well is carried out to hip treatment, and hip temperature is 1200 ℃, and pressure is 130MPa, and the time is 2 hours, and after processing, the density of target ingot blank is 7.61g/cm
3, be 99.5% of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-33Cr-11Pt-11SiO2 (at%).
Embodiment 5
The material powder of selecting is Co, Cr, Pt, CoO, Cr
2o
3, six kinds of powder of Si, wherein the content of Co is 47at%, the content of Cr is 15at%, the content of Pt is 15at%, the content of Si is 15at%, the content of CoO is 6at%, Cr
2o
3content be 2at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is agate ball, and ratio of grinding media to material is 15:1, and the mixed powder time is 30 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 180MPa, and the dwell time is 0.5 hour, forms target ingot blank; Be evacuated to subsequently 3x10
-3pa, then fill Ar gas to 6Pa, at 1000 ℃, to carry out solid phase reaction and synthesize, the time is 3 hours, after processing, the density of target ingot blank is 7.36g/cm
3, be 95.8% of solid density, SiO
2particle size distribution scope is 100～550nm, and average grain diameter is 205nm; The target of handling well is carried out to hip treatment, and hip temperature is 1300 ℃, and pressure is 130MPa, and the time is 2 hours, and after processing, the density of target ingot blank is 7.65g/cm
3, be 99.6% of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-19Cr-15Pt-15SiO
2(at%).
Embodiment 6
The material powder of selecting is Co, Cr, Pt, Co
2o
3, Cr
2o
3, six kinds of powder of Si, wherein the content of Co is 48at%, the content of Cr is 22at%, the content of Pt is 15at%, the content of Si is 9at%, Co
2o
3content be 4at%, Cr
2o
3content be 2at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is steel ball, and ratio of grinding media to material is 20:1, and the mixed powder time is 24 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 100MPa, and the dwell time is 1 hour, forms target ingot blank; Be evacuated to subsequently 8x10
-3pa, then fill Ar gas to 8Pa, at 1000 ℃, to carry out solid phase reaction and synthesize, the time is 2.5 hours, after processing, the density of target ingot blank is 8.26g/cm
3, be 95.7% of solid density, SiO
2particle size distribution scope is 350～950nm, and average grain diameter is 440nm; The target of handling well is carried out to hip treatment, and hip temperature is 1200 ℃, and pressure is 140MPa, and the time is 2 hours, and after processing, the density of target ingot blank is 8.56g/cm
3, be 99.2% of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-25Cr-14Pt-8SiO
2(at%).
Embodiment 7
The material powder of selecting is Co, Cr, Pt, Cr
2o
3, Co
2o
3, CoO, seven kinds of powder of Si, wherein the content of Co is 49at%, the content of Cr is 21at%, the content of Pt is 12at%, the content of Si is 10at%, Cr
2o
3content be 4at%; Co
2o
3content be 2at%, the content of CoO is 2at%; Adopt subsequently planetary ball mill mode to mix powder, employing medium ball is steel ball, and ratio of grinding media to material is 14:1, and the mixed powder time is 36 hours; Adopt hydraulic press to carry out pre-molding in the powder mixing subsequently, pressure is 200MPa, and the dwell time is 1 hour, forms target ingot blank; Be evacuated to subsequently 1x10
-3pa, then fill Ar gas to 20Pa, at 1000 ℃, to carry out solid phase reaction and synthesize, the time is 3 hours, after processing, the density of target ingot blank is 7.78g/cm
3, be 96.6% of solid density, SiO
2particle size distribution scope is 100～450nm, and average grain diameter is 170nm; The target of handling well is carried out to hip treatment, and hip temperature is 1300 ℃, and pressure is 140MPa, and the time is 4 hours, and after processing, the density of target ingot blank is 8.03g/cm
3, be 99.8% of solid density; Finally carry out mechanical process and obtain needing the target product of size, target finally consist of Co-27Cr-11Pt-9SiO
2(at%).
Claims (7)
1. a Co-Cr-Pt-SiO
2the preparation method of target, is characterized in that, following processing technology step, consists of:
(1) selecting Co, Cr, Pt, Si and oxide is material powder; Wherein the content of Co is 45～65at%, and the content of Cr is 12～35at%, and the content of Pt is 3～20at%, and the content of Si is 4～15at%, and the content of oxide is 2～20at%;
(2) material powder is mixed, hybrid mode is planetary ball mill, and employing medium ball is steel ball, agate ball or zirconia ball, and ratio of grinding media to material is 5:1～20:1, and the mixed powder time is 12～36 hours;
(3) after mixed powder, adopting hydraulic press to carry out pre-molding, is under 10～200MPa, to carry out the pre-molding of 0.5～2 hour at pressure;
(4) the target ingot blank of handling well in step (3) is evacuated to 1x10
-2～1x10
-3pa, then fill Ar gas to 1～20Pa, at 850～1000 ℃, to carry out solid phase reaction and synthesize, the time is 1～4 hour;
(5) target of handling well in step (4) is carried out to hip treatment, hip temperature is 1000～1500 ℃, and pressure is 100～150MPa, and the time is 1～16 hour;
(6) carry out the target product that mechanical process obtains needing size.
2. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, described oxide is Co
3o
4, CoO, Co
2o
3, Cr
2o
3in one or more mixture.
3. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, target ingot blank is in carrying out solid phase reaction building-up process, and oxide reacts with Si powder and generates SiO
2.
4. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, target ingot blank carry out solid phase reaction synthetic after, density can reach the more than 95% of solid density.
5. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, target ingot blank is carrying out the synthetic rear SiO generating of solid phase reaction
2particle is tiny, and its particle size distribution is 100～1000nm.
6. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, described material powder purity is all more than or equal to 99.95wt%.
7. a kind of Co-Cr-Pt-SiO according to claim 1
2the preparation method of target, is characterized in that, described material powder Co, Cr, Pt, Si powder size are 1～50 μ m, and oxide granularity is 1～10 μ m.
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|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060233658A1 (en) * | 2005-04-18 | 2006-10-19 | Heraeus, Inc., A Corporation Of The State Of Arizona | Enhanced formulation of cobalt alloy matrix compositions |
| CN1880501A (en) * | 2005-06-15 | 2006-12-20 | 黑罗伊斯公司 | Enhanced oxide-containing sputter target alloy compositions |
| CN1884611A (en) * | 2005-06-24 | 2006-12-27 | 黑罗伊斯有限公司 | Enhanced oxygen non-stoichiometry compensation for thin films |
| CN1952207A (en) * | 2005-04-19 | 2007-04-25 | 黑罗伊斯有限公司 | Enhanced multi-component oxide-containing sputter target alloy compositions |
| US20070134124A1 (en) * | 2002-07-23 | 2007-06-14 | Heraeus Incorporated | Sputter target and method for fabricating sputter target including a plurality of materials |
-
2014
- 2014-08-12 CN CN201410394572.2A patent/CN104174851B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070134124A1 (en) * | 2002-07-23 | 2007-06-14 | Heraeus Incorporated | Sputter target and method for fabricating sputter target including a plurality of materials |
| US20060233658A1 (en) * | 2005-04-18 | 2006-10-19 | Heraeus, Inc., A Corporation Of The State Of Arizona | Enhanced formulation of cobalt alloy matrix compositions |
| CN1952207A (en) * | 2005-04-19 | 2007-04-25 | 黑罗伊斯有限公司 | Enhanced multi-component oxide-containing sputter target alloy compositions |
| CN1880501A (en) * | 2005-06-15 | 2006-12-20 | 黑罗伊斯公司 | Enhanced oxide-containing sputter target alloy compositions |
| CN1884611A (en) * | 2005-06-24 | 2006-12-27 | 黑罗伊斯有限公司 | Enhanced oxygen non-stoichiometry compensation for thin films |
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|---|---|
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