CN103510055B - The preparation method of high-purity copper target material - Google Patents
The preparation method of high-purity copper target material Download PDFInfo
- Publication number
- CN103510055B CN103510055B CN201210223059.8A CN201210223059A CN103510055B CN 103510055 B CN103510055 B CN 103510055B CN 201210223059 A CN201210223059 A CN 201210223059A CN 103510055 B CN103510055 B CN 103510055B
- Authority
- CN
- China
- Prior art keywords
- purity copper
- copper target
- target material
- purity
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
A preparation method for high-purity copper target material, comprising: first carry out preheating to high-purity copper ingot; Then first time thermal treatment is carried out after the high-purity copper ingot in described warm being forged; Then the high-purity copper ingot after first time thermal treatment is rolled, form copper coin material and carry out second time thermal treatment, form copper target blank; Finally mechanical workout is carried out to described copper target blank, form high-purity copper target material.Adopt technical scheme of the present invention, grain-size can be produced and be less than 100 microns and sputter direction preferably high-purity copper target material.
Description
Technical field
The present invention relates to semi-conductor sputtering field, particularly relate to a kind of preparation method of high-purity copper target material.
Background technology
Sputtering target material manufactures the extremely important critical material of the necessary one of semi-conductor chip, the principle of its making devices is utilized to be adopt physical gas phase deposition technology (PVD), gas ion bombardment target is accelerated with high pressure, the atom of target is sputtered out, deposit in the form of a film on silicon chip, the final distribution structure forming complexity in semi-conductor chip.Sputtering target material has the many advantages such as homogeneity, controllability of metal coating, is widely used in semiconductor applications.Along with developing rapidly of semicon industry, compared with conventional interconnect materials of aluminum, because copper has higher specific conductivity and better electromigration resistance properties, so be widely used at present in the interconnection line of super large-scale integration, copper sputtering target material has become semicon industry and has developed indispensable critical material.
But grain-size, the grain orientation of target have a great impact the preparation of integrated circuit metal film and performance.Be mainly manifested in: 1. along with the increase of grain-size, film deposition rate is tending towards reducing; 2. in suitable grain size range, plasma impedance when target uses is lower, and film deposition rate is high and film gauge uniformity is good; 3., for improving the performance of target, while controlling target crystalline grains size, also strictly must control the grain orientation of target, be easily splashed to make it and treat on sputtering substrate.
Based on These characteristics, little to grain-size in industry, particularly, grain-size is less than 100 microns and the good copper target in sputter procedure target as sputter direction has certain demand.For this demand of semicon industry, the preparation method of traditional copper target cannot meet.
For the problems referred to above, the preparation method that the present invention proposes a kind of new high-purity copper target material solves.
Summary of the invention
The problem that the present invention solves is the preparation method proposing a kind of new high-purity copper target material, produces grain-size and is less than 100 microns and sputter direction preferably high-purity copper target material.
For solving the problem, the present invention proposes a kind of preparation method of high-purity copper target material, comprising:
Preheating is carried out to high-purity copper ingot;
High-purity copper ingot in described warm is forged;
First time thermal treatment is carried out to the described high-purity copper ingot through forging;
High-purity copper ingot after first time thermal treatment is rolled, forms copper coin material;
Second time thermal treatment is carried out to described copper coin material, forms copper target blank;
Mechanical workout is carried out to described copper target blank, forms high-purity copper target material.
Alternatively, the temperature of described preheating is 300 DEG C ~ 700 DEG C.
Alternatively, described first time, heat treated temperature was 200 DEG C ~ 500 DEG C, and soaking time is 1 hour ~ 4 hours.
Alternatively, the heat treated temperature of described second time is 200 DEG C ~ 450 DEG C, and soaking time is 1 hour ~ 3 hours.
Alternatively, the pressure range of described calendering is 500 tons ~ 1600 tons.
Alternatively, before mechanical workout is carried out to described copper target blank, also described copper target blank is flattened.
Alternatively, described calendaring processes carries out repeatedly.
Alternatively, after each calendaring processes, all the second heat treatment step is carried out to described copper coin material.
Compared with prior art, the present invention has the following advantages: first carry out preheating to high-purity copper ingot and forge the high-purity copper ingot in warm, the crystal grain that preliminary destruction is thick; Then carrying out first time thermal treatment to the described high-purity copper ingot through forging, namely carrying out thermal stresses release to the high-purity copper ingot after forging, making crystal grain miniaturization, grain orientation rationalizes; Roll the high-purity copper ingot after first time thermal treatment afterwards, form copper coin material and carry out second time thermal treatment to described copper coin material, form copper target blank, said process makes the further miniaturization of crystal grain by extruding, and grain orientation rationalizes further; Finally mechanical workout is carried out to described copper target blank, form high-purity copper target material, to meet the different size demand that semi-conductor sputtering uses.
In possibility, first time, heat treated temperature was 200 DEG C ~ 500 DEG C, and soaking time is 1 hour ~ 4 hours, the too low crystal grain easily making to be destroyed of temperature not easily crystallization nucleation, temperature is too high makes the grain growing of nucleation too much, does not meet the requirement of crystal grain miniaturization; Soaking time is long also can cause the grain growing of nucleation excessive, and the too short meeting of soaking time causes high-purity copper ingot internal/external heating uneven.
In possibility, the pressure range of calendering is 500 tons ~ 1600 tons, and pressure is crossed conference and caused grain orientation flat, is unfavorable in sputter procedure, and to the control in this target as sputter direction, too small meeting makes crystal grain miniaturization not reach requirement.
In possibility, the heat treated temperature of second time is 200 DEG C ~ 450 DEG C, and soaking time is 1 hour ~ 3 hours, and the too low thermal stresses generated in calender line that easily causes of temperature cannot discharge, temperature is too high makes the grain growing of nucleation too much, does not meet the requirement of crystal grain miniaturization; Soaking time is long also can cause the grain growing of nucleation excessive, and the too short meeting of soaking time causes copper coin material internal/external heating uneven.
Accompanying drawing explanation
Fig. 1 is preparation method's schematic flow sheet of the high-purity copper target material of the present embodiment;
Fig. 2 is the schematic diagram forging technique direction of travel in the present embodiment;
Fig. 3 is the crystalline network schematic diagram of copper.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Because the present invention focuses on interpretation principle, therefore, chart not in scale.
Figure 1 shows that the schema of the preparation method of the high-purity copper target material that the present embodiment provides, Fig. 2 forges structural representation corresponding to technique in Fig. 1.Below be specifically introduced.
Perform step S11, preheating is carried out to high-purity copper ingot.
The general purity requirement of semiconductor copper target is at 3N(99.99%) more than, be such as 4N5(99.995%) or 5N(99.999%).So the purity of high-purity copper ingot used is 4N(99.99%) more than, in the present embodiment be preferably 4N5(99.995%) copper ingot.In the present embodiment, the preferred cubes of shape of described high-purity copper ingot, its size can carry out cutting off to reach the size being easy to subsequent disposal through sawing machine on starting material basis.In other embodiment, the shape of high-purity copper ingot also can be right cylinder.
Carry out thermal pretreatment to high-purity copper ingot before forging, the mode of described thermal pretreatment is for be heated to 300 DEG C ~ 700 DEG C by high-purity copper ingot.In this temperature range, high-purity copper ingot entirety is made to be beneficial to follow-up forging.Particularly, the words that temperature is too high, the grain-size of the generation of recrystallize can be caused larger, make the last target formed can not meet the requirement of semi-conductor sputtering, and the temperature of preheating is too low or do not carry out the words of preheating, follow-up forging will be carried out not too easy, is not fine for improving the effect of high-purity copper ingot internal performance aspect, and high-purity copper ingot easily crackle occurs forging in process.If the overlong time of insulation, then can cause the grain-size of the generation of copper ingot recrystallize larger; If the time of insulation is too short, then high-purity copper ingot internal/external heating can be made uneven.
Then, perform step S12, the high-purity copper ingot in described warm is forged, then carries out first time thermal treatment.
The described embodiment forged is utilize air hammer to impact along the surface of high-purity copper ingot high-purity copper ingot.The effect forged original thick dendritic particles and columnar grain is smashed become small grains, make original segregation in high-purity copper ingot, loose, pore, slag inclusion etc. are compacted and seam, its tissue becomes more tight, improves plasticity and the mechanical property of high-purity copper ingot.
Consider that copper is face-centred cubic structure, thus in this step in order to as early as possible by thick crystal grain destroy, forge to divide and carry out for three times, as shown in Figure 2, at every turn respectively to carry out (X-direction, Y-direction or Z-direction) along a direction, and the direction forged for three times is vertical between two.
Described high-purity copper ingot through forging is carried out first time thermal treatment, and described first time, heat treated temperature was 200 DEG C ~ 500 DEG C, and soaking time is 1 hour ~ 4 hours, the present embodiment, and preferred temperature is 250 DEG C, and holding time is 2 hours.In the first time that the present embodiment provides heat treated temperature range, the crystal grain forging rear fragmentation is carried out recrystallize (recrystallization temperature of copper is 200 DEG C ~ about 280 DEG C), the too low crystal grain easily making to be destroyed of temperature not easily crystallization nucleation, temperature is too high makes the grain growing of nucleation too much, does not meet the requirement of crystal grain miniaturization; Soaking time is long also can cause the grain growing of nucleation excessive, and the too short meeting of soaking time causes high-purity copper ingot internal/external heating uneven.
Comparatively optimize, described first time thermal treatment can be carried out under vacuum, and the high-purity copper ingot by forging can be prevented to be oxidized under the condition of high temperature.
Then, perform step S13, after described first time thermal treatment, high-purity copper ingot is rolled, form copper coin material, then carry out second time thermal treatment, form copper target blank.
Because first time heat treated temperature can not make the grain growing of nucleation excessive, this temperature is applicable to again carrying out viscous deformation to copper, based on this, rolls immediately after first time thermal treatment to high-purity copper ingot.
Copper is face-centred cubic structure, as shown in Figure 3, respectively there is an atom in eight drift angles and six faces, in the magnetron sputtering process of target, grain orientation is that sputtered out its sputter direction rear of the atom in crystal orientation (111) is easy to reach by sputter substrate, this step, by suitable pressure, controls the crystal grain content raising that high-purity copper target material forms crystal orientation (111).In pressure-controlling, the present inventor finds, pressure is crossed conference and caused grain orientation flat, and the too small meeting of pressure makes crystal grain miniaturization not reach requirement.In this step, preferably, carrying out rolling preferred pressure range to high-purity copper ingot is that rolling press in 500 tons ~ 1600 tons is implemented to reach 60% ~ 80% to control high-purity copper target material formation crystal orientation (111) proportion.
The embodiment of calender line is: the overflow mould high-purity copper ingot being placed in calender device (such as forging press, air hammer or rolling press) carries out extrusion molding.Described calendering can adopt forward extrusion, and namely the direction of extrusion of calender device is consistent with the flow direction of high-purity copper ingot, also can adopt reverse extrusion, and namely the direction of extrusion of calender device is contrary with the flow direction of high-purity copper ingot.In the present embodiment, adopt forward hot extrusion, namely the direction of extrusion of calender device is consistent with the flow direction of high-purity copper ingot, and calendering is carried out at a certain temperature, the calendering of the present embodiment is carried out after heat treatment immediately, if temperature is too low, the internal and external temperature of high-purity copper ingot is uneven, easily cracks during extruding.
The size of the determined copper coin material of shape and size of calendering mould.
By the crimp rate that conservative control extrusion temperature is suitable with setting, accurately can control the compact dimensions precision of copper coin material, realize further crystal grain thinning and reduce the object of target material surface roughness, prepare for producing the target that meets plastic deformation process requirement.
Afterwards, second time thermal treatment is carried out to copper coin material, form copper target blank.
The heat treated temperature of described second time is 200 DEG C ~ 450 DEG C, and soaking time is 1 hour ~ 3 hours, the present embodiment, and preferred temperature is 250 DEG C, and holding time is 2 hours.In the heat treated temperature range of second time that the present embodiment provides, by the thermal stresses release generated in calender line, the too low thermal stresses generated in calender line that easily causes of temperature cannot discharge, and temperature is too high makes the grain growing of nucleation too much, does not meet the requirement of crystal grain miniaturization; Soaking time is long also can cause the grain growing of nucleation excessive, and the too short meeting of soaking time causes copper coin material internal/external heating uneven.
After above-mentioned steps completes, the sample intercepting a small volume from copper target blank carries out the detection of grain size, grain orientation, if meet the demands both above-mentioned, then carries out next step S14; If brilliant excessive, grain orientation does not also reach sputter direction control overflow, then perform this step S13 many times until grain size, grain orientation meet the demands.
Perform step S14, described copper target blank is flattened.
Leveling in this step by first detecting the planeness on the surface of copper target blank, if planeness meets the requirements, then can perform step S15; If planeness is undesirable, then correct protruding the fulcrum mode of exerting pressure downwards, also can according to the planeness on the surface of copper target blank, make the apparatus for correcting that fluctuating curved surface concavo-convex with it have the curved surface of counter undulations and correct.
Perform step S15, mechanical workout is carried out to described copper target blank, form high-purity copper target material.
This step comprises the technique such as roughing, precision work, make satisfactory target product, wherein roughing can take out circular copper target by the method for Linear cut from square copper target blank, then precision work is carried out to the copper target of described circle, for product size turning, comprise border Linear cut, lower planes grinding machine is processed.Target material surface form accuracy is made to meet target requirement.
The present invention is mainly through controlling viscous deformation (temperature forged and calender pressure), heat treated temperature, time, and the method that the heat treatment phase under viscous deformation repeatedly and specified temp combines realizes making the copper target meeting semi-conductor sputtering copper target crystalline grains and require to require with grain orientation, the grain-size obtaining copper target is 30 μm ~ 100 μm, and grain orientation (111) proportion reaches the high-purity copper target material of 60% ~ 80%.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong to the protection domain of technical solution of the present invention.
Claims (6)
1. a preparation method for high-purity copper target material, is characterized in that, comprising:
Preheating is carried out to high-purity copper ingot;
High-purity copper ingot in described warm is forged;
Carry out first time thermal treatment to the described high-purity copper ingot through forging, described first time, heat treated temperature was 200 DEG C ~ 500 DEG C, and soaking time is 1 hour ~ 4 hours;
Roll the high-purity copper ingot after first time thermal treatment immediately, form copper coin material, the pressure range of described calendering is 500 tons ~ 1600 tons;
Second time thermal treatment is carried out to described copper coin material, forms copper target blank;
Mechanical workout is carried out to described copper target blank, forms high-purity copper target material.
2. the preparation method of high-purity copper target material according to claim 1, is characterized in that, the temperature of described preheating is 300 DEG C ~ 700 DEG C.
3. the preparation method of high-purity copper target material according to claim 1, is characterized in that, the heat treated temperature of described second time is 200 DEG C ~ 450 DEG C, and soaking time is 1 hour ~ 3 hours.
4. the preparation method of high-purity copper target material according to claim 1, is characterized in that, before carrying out mechanical workout, also flattens described copper target blank described copper target blank.
5. the preparation method of high-purity copper target material according to claim 1, is characterized in that, described calendaring processes carries out repeatedly.
6. the preparation method of high-purity copper target material according to claim 5, is characterized in that, after each calendaring processes, all carry out the second heat treatment step to described copper coin material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210223059.8A CN103510055B (en) | 2012-06-27 | 2012-06-27 | The preparation method of high-purity copper target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210223059.8A CN103510055B (en) | 2012-06-27 | 2012-06-27 | The preparation method of high-purity copper target material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103510055A CN103510055A (en) | 2014-01-15 |
| CN103510055B true CN103510055B (en) | 2015-10-21 |
Family
ID=49893476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210223059.8A Active CN103510055B (en) | 2012-06-27 | 2012-06-27 | The preparation method of high-purity copper target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103510055B (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107953084B (en) * | 2017-11-24 | 2019-08-13 | 韶关市欧莱高新材料有限公司 | A kind of manufacturing method of rafifinal rotary target material |
| CN111195803A (en) * | 2018-11-17 | 2020-05-26 | 上海派尼科技实业股份有限公司 | Method for preparing target plate |
| CN111197148B (en) * | 2018-11-20 | 2021-11-19 | 宁波江丰电子材料股份有限公司 | Method for manufacturing target material |
| CN110241392B (en) * | 2019-07-16 | 2021-08-17 | 宁波江丰电子材料股份有限公司 | Target material, method for improving utilization rate of target material and application |
| CN111451314B (en) * | 2020-04-01 | 2021-02-26 | 东莞市欧莱溅射靶材有限公司 | Preparation method of high-purity copper rotary target |
| JP7309217B2 (en) * | 2020-06-26 | 2023-07-18 | オリエンタル コッパー シーオー．エルティーディー． | Method for manufacturing copper cylindrical targets for thin film coating using sputtering method from hot extrusion technology |
| CN112170753B (en) * | 2020-08-27 | 2022-05-31 | 金嘉品（昆山）金属工业有限公司 | Semiconductor copper back target processing method |
| CN112323028A (en) * | 2020-11-11 | 2021-02-05 | 广安市立正金属有限公司 | Non-smelting casting method for high-purity copper |
| CN112680626B (en) * | 2020-12-09 | 2022-12-02 | 爱发科电子材料（苏州）有限公司 | Preparation process of copper-aluminum-silicon alloy target material for integrated circuit |
| CN113652654B (en) * | 2021-08-11 | 2023-08-18 | 宁波江丰电子材料股份有限公司 | Deformation-resistant oxygen-free copper backboard and preparation method thereof |
| CN113649509B (en) * | 2021-08-13 | 2024-03-22 | 宁波江丰电子材料股份有限公司 | Copper target and preparation method thereof |
| CN113774346A (en) * | 2021-09-08 | 2021-12-10 | 宁波江丰电子材料股份有限公司 | Oxygen-free copper backboard and preparation method thereof |
| CN113817995B (en) * | 2021-09-17 | 2023-09-08 | 宁波江丰电子材料股份有限公司 | High-purity copper target and preparation method thereof |
| CN113857402B (en) * | 2021-09-27 | 2024-05-24 | 宁波江丰电子材料股份有限公司 | Preparation method of alloy high-purity copper target |
| CN114000072A (en) * | 2021-10-28 | 2022-02-01 | 宁波江丰电子材料股份有限公司 | Heat treatment method of copper back plate |
| CN116240474B (en) * | 2023-03-21 | 2023-10-20 | 山东海特电子材料有限公司 | Preparation method of high-purity copper target |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509125A (en) * | 2009-03-19 | 2009-08-19 | 金川集团有限公司 | Method for producing copper sputtering target material |
| CN102146554A (en) * | 2011-03-16 | 2011-08-10 | 杭州宣宁电子材料有限公司 | Preparation method for high-purity copper sputtering target material |
| CN102418058A (en) * | 2011-12-02 | 2012-04-18 | 宁波江丰电子材料有限公司 | Manufacturing method for nickel target billet and nickel target material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001049426A (en) * | 1999-07-08 | 2001-02-20 | Praxair St Technol Inc | Manufacture of copper sputtering target, and assembly of copper sputtering target and backing plate |
-
2012
- 2012-06-27 CN CN201210223059.8A patent/CN103510055B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509125A (en) * | 2009-03-19 | 2009-08-19 | 金川集团有限公司 | Method for producing copper sputtering target material |
| CN102146554A (en) * | 2011-03-16 | 2011-08-10 | 杭州宣宁电子材料有限公司 | Preparation method for high-purity copper sputtering target material |
| CN102418058A (en) * | 2011-12-02 | 2012-04-18 | 宁波江丰电子材料有限公司 | Manufacturing method for nickel target billet and nickel target material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103510055A (en) | 2014-01-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103510055B (en) | The preparation method of high-purity copper target material | |
| CN102517531B (en) | Method for preparing high-purity tantalum target | |
| CN111197148B (en) | Method for manufacturing target material | |
| CN102517550B (en) | High purity tantalum target and preparation process thereof | |
| JP4327460B2 (en) | Refractory metal plate having uniform texture and method for producing the plate | |
| CN103572223B (en) | The manufacture method of tantalum target and tantalum target assembly | |
| CN104419901B (en) | A kind of manufacture method of tantalum target | |
| CN111088481A (en) | Nickel target blank and method for manufacturing target material | |
| CN112453088B (en) | Method for refining crystal grains in ultra-high pure copper or copper alloy | |
| JP4405606B2 (en) | Titanium sputtering target and manufacturing method thereof | |
| CN111254398B (en) | Platinum sputtering target with high oriented grain and preparation method thereof | |
| CN103184419A (en) | Production method of aluminum-neodymium alloy target material | |
| CN114411104A (en) | High-purity silver target and preparation method and application thereof | |
| CN107119244A (en) | A kind of preparation method of high preferred orientation fine grain ultra-pure aluminum target | |
| KR20080113124A (en) | Copper target | |
| CN102424940A (en) | Preparation method for high-purity cobalt target | |
| CN103898459B (en) | A kind of preparation method of high-purity cobalt target | |
| CN113755801A (en) | Preparation method of high-purity aluminum target material with uniform orientation | |
| CN104726829A (en) | High purity NiPt alloy target material and preparation method thereof | |
| CN104694862B (en) | Preparation method of silver sputtering target blank | |
| CN113817995A (en) | High-purity copper target material and preparation method thereof | |
| CN108465700B (en) | Tantalum plate rolling method for obtaining sputtering target material with uniform structure and texture | |
| CN102350439A (en) | Hot rolling method for nickel target billet used for semiconductor | |
| CN102091733B (en) | Manufacturing method of high-purity copper targets | |
| CN111304608A (en) | Nickel-platinum alloy sputtering target with high oriented crystal grains and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 315400 Ningbo City, Yuyao Province Economic Development Zone, state science and Technology Industrial Park Road, No. 198, No. Applicant after: NINGBO JIANGFENG ELECTRONIC MATERIAL CO., LTD. Address before: 315400 Ningbo City, Yuyao Province Economic Development Zone, state science and Technology Industrial Park Road, No. 198, No. Applicant before: Ningbo Jiangfeng Electronic Materials Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |