CN1104758A - Crucible with titanium diboride coating and its manufacture - Google Patents
Crucible with titanium diboride coating and its manufacture Download PDFInfo
- Publication number
- CN1104758A CN1104758A CN 94115523 CN94115523A CN1104758A CN 1104758 A CN1104758 A CN 1104758A CN 94115523 CN94115523 CN 94115523 CN 94115523 A CN94115523 A CN 94115523A CN 1104758 A CN1104758 A CN 1104758A
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- crucible
- titanium diboride
- deposited
- coating
- wall surface
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Abstract
The crucible for smelting metal used in vacuum plating has a crucible body with recesses whose internal wall is coated by TiB. Al2O3 or SiO2 as insulating protection layer is coated onto the upper surface of the crucible wall. It features electric conducting, molter metal corrosion resistance, and long service life.
Description
The present invention relates to a kind of improved crucible, particularly a kind of vacuum coating or plated film deposite metal crucible simultaneously, also relate to a kind of method of making crucible.
At present the used crucible in deposite metal mostly is tungsten, molybdenum, tantalum etc. refractory metal is made and does in the vacuum evaporator, because the metal generation reaction or alloying or the fusion that are melted metal and make crucible, the metal of making crucible is rapidly by etch, and the metal or the vapor-deposited film that are melted are contaminated.Oxide, nitride crucible or its composite crucible can be avoided and some metal reaction, thereby improve plated film clarity and crucible life, see " membrane science and technical manual " first volume that China Machine Press published in 1991.But this class crucible poorly conductive, be unsuitable for doing the electrode crucible, because oxide wherein and nitride mostly are electrically non-conductive material or insulating materials, see " the ceramic introduction " the 909th page that China Construction Industry Press published in 1987, make the electrode crucible if adopt water jacketed copper crucible, then power consumption is big, and plated film speed is low.
The purpose of this invention is to provide a kind of can the conduction, can improve anti-molten metal attack again, and the crucible that scribbles titanium diboride coating of long service life.
Another object of the present invention provides a kind of preparation and can conduct electricity, and can improve anti-molten metal attack again, and the method that scribbles the titanium diboride coating crucible of long service life.
In order to realize one of foregoing invention purpose; the present invention scribbles the crucible of titanium diboride coating; refractory metal crucible body with a band groove; its characteristics are: be coated with titanium diboride coating on the inwall of described crucible groove, partly or entirely be coated with alundum (Al or silicon dioxide insulator protective layer in the top wall surface of described crucible body.
The thickness range that is coated on the titanium diboride coating on the described crucible groove inwall is 0.2～2mm.
Being coated on the alundum (Al of described crucible top wall surface or the thickness range of silicon dioxide insulator protective layer is: 0.1～1.0mm.
Here the refractory metal of indication is the metal that tungsten, molybdenum, tantalum etc. are fit to do crucible.
Employing tungsten has been described in the background technology of front, molybdenum, refractory metals such as tantalum can be used as the crucible of fusing than low-melting-point metal, but can produce reaction with the intermetallic of manufacturing crucible owing to be melted metal, or alloying or fusion, and the refractory metal crucible is etched rapidly, pot life is short, make deposite metal or evaporated metal contaminated, and oxide, though nitride crucible or its composite crucible can overcome above-mentioned deficiency, but its poorly conductive is unsuitable for doing the electrode crucible, and selects for use titanium diboride to make crucible coating layer, its reason is that titanium diboride has the fusing point height, reach 2930 ℃, conduct electricity very well, ρ
Room temperature=12 μ ncm, and chemical stability is good, advantages such as wearability is strong, the refractory metal crucible that scribbles titanium diboride itself can be used as negative electrode or the anode in the electrode, thereby crucible of the present invention can be conducted electricity, and don't can manufacture between the metal of crucible and institute deposite metal and produce reaction, alloying or fusion, and as copper crucible, need need not water-cooled.
Top wall surface at crucible scribbles insulating protective layers such as alundum (Al or silica, is in order to guarantee under the situation of crucible as electrode, prevents the starting the arc of crucible outer and pollutes the metal or alloy that is melted, and can prolong the life-span of described crucible simultaneously.
In order to realize another object of the present invention, the present invention's preparation scribbles the method for titanium diboride coating, comprises following several steps:
(a) get the crucible body that the refractory metal that is suitable for doing crucible is processed into the band groove;
(b) titanium diboride is coated on the inwall of described crucible groove, until being deposited on till titanium diboride on the crucible groove inwall reaches desired thickness; With
(c) alundum (Al or silica partly or entirely are coated on the top wall surface of described crucible, till the alundum (Al that is deposited on the crucible top wall surface or silica reach desired thickness.
Here to be deposited on the desired thickness of titanium diboride coating on the described crucible groove inwall be 0.2～2mm to indication.
The alundum (Al or the desired thickness of silica that are deposited on described crucible top wall surface are: 0.1～1.0mm.
Compared with prior art, the advantage of crucible of the present invention is:
(1) the molten-metal-resistant aggressivity is good, because crucible of the present invention adopts titanium diboride to make the groove inside coating, the titanium diboride fusing point is up to 2930 ℃, and chemical stability is good, wearability is good, titanium diboride coating can not produce reaction, alloying or fusion with being melted intermetallic, so the anti-molten metal attack of crucible of the present invention is good.
(2) good conductivity, the electricalresistivity of titanium diboride
Room temperatureTherefore=12 μ n cm are body with the refractory metal, are that the crucible of coating has good electrical conductivity with the titanium diboride.
(3) need not water-cooled, the present invention compares with the copper crucible that adopts water-cooled, and power consumption is low, plated film purity height.
(4) long service life, when using tungsten, molybdenum or graphite to make electrode crucible evaporation metal nickel, the content of tungsten, molybdenum or carbon is higher in the plated film, crucible only uses several times, and when using crucible nickel plating of the present invention, plated film purity height, impurity content is low, and crucible can use tens times to tens times.
Below in conjunction with accompanying drawing crucible of the present invention is further described.
Fig. 1 is that the master of crucible of the present invention looks generalized section.
Fig. 1 represents a kind of crucible that has titanium diboride coating; on the inwall of the groove of refractory metal crucible body 3, apply titanium diboride coating 2, partly or entirely apply alundum (Al or silicon dioxide insulator protective layer 1 in the top wall surface of described refractory metal crucible body 3.
The specific embodiment that the present invention's preparation has titanium diboride coating is:
(1) get the crucible body that tungsten, molybdenum or tantalum are processed into the band groove, its size and shape are decided according to concrete purposes,
(2) use E44 epoxy resin with titanium diboride powder furnishing pasty state, the weight ratio of epoxy resin and titanium diboride is 0.1～1,
(3) crucible groove inwall is sprayed noisy, cleaning, makes its inwall be oily, the dustless hair side of nothing,
(4) the pasty state titanium diboride is coated on the crucible inwall, its thickness is 0.2～2mm as required.
(5) treat that the pasty state titanium diboride coating after crucible groove inwall solidifies, carries out vacuum high-temperature sintering again, make the organic matter volatilization, be warming up to 1300 ℃ of sintering then 1～4 hour,
(6) top wall surface at crucible partly or entirely applies alundum (Al or silica slurry, and its thickness is as required: 0.1～1.0mm.
(7) treat alundum (Al or silica slurry air dry after, through vacuum high-temperature oven dry or atmosphere hyperthermia drying, wherein bake out temperature is 300～800 ℃ again, the time is 0.5～2 hour.
During (8) if necessary as the electrode crucible, all apply alundum (Al or silicon dioxide insulator protective layer, then should remove described insulating protective layer at the position that connects power supply in described crucible top wall surface.
According to above-mentioned concrete implementation step, prepared three batches of crucibles, the composition of three batches of crucibles is as shown in table 1, and the performance of three batches of crucibles is as shown in table 2.
The concrete composition of table 1 embodiment crucible
The performance of table 2 embodiment crucible
Annotate (1) electric conductivity with universal meter test crucible, red test pencil is at crucible body bottom surface point, and black meter pen slides at the crucible inwall, records two resistance between the nib.
(2) test insulating barrier insulating properties method is the same, and just black meter pen slides on insulating barrier.
(3) service life of crucible, can be regarded as once with vacuum arc evaporation 10 gram nickel.
Claims (6)
1, a kind of crucible that scribbles titanium diboride coating; refractory metal crucible body with a band groove; it is characterized in that: be coated with titanium diboride coating on the groove inwall of described crucible, partly or entirely be coated with three oxygen, two aluminium or silicon dioxide insulator protective layer in the top wall surface of described crucible body.
2, crucible according to claim 1 is characterized in that: the titanium diboride coating thickness that is coated on the described crucible groove inwall is: 0.2～2mm.
3, crucible according to claim 1 is characterized in that: remove and to be overlying on the alundum (Al of described crucible top wall surface or the thickness of silicon dioxide insulator protective layer is: 0.1～1.0mm.
4, a kind of with preparing the method that scribbles the titanium diboride coating crucible, comprise following several steps:
(a) get the crucible body that the refractory metal that is suitable for doing crucible is processed into the band groove;
(b) titanium diboride is deposited on the inwall of described crucible groove, until being deposited on till titanium diboride on the crucible groove inwall reaches desired thickness; With
(c) alundum (Al or silica partly or entirely are deposited on the top wall surface of described crucible, till the alundum (Al that is deposited on the crucible top wall surface or silica reach desired thickness.
5, method according to claim 4 is characterized in that: the desired thickness of titanium diboride coating that is deposited on the described crucible groove inwall is: 0.2～2mm.
6, method according to claim 4 is characterized in that: the alundum (Al or the desired thickness of silica dioxide coating that are deposited on described crucible top wall surface are: 0.1～1.0mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94115523A CN1039247C (en) | 1994-09-10 | 1994-09-10 | Crucible with titanium diboride coating and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94115523A CN1039247C (en) | 1994-09-10 | 1994-09-10 | Crucible with titanium diboride coating and its manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1104758A true CN1104758A (en) | 1995-07-05 |
| CN1039247C CN1039247C (en) | 1998-07-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94115523A Expired - Fee Related CN1039247C (en) | 1994-09-10 | 1994-09-10 | Crucible with titanium diboride coating and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1039247C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457966C (en) * | 2002-09-03 | 2009-02-04 | 三星Sdi株式会社 | Heating crucible for organic film forming squipment |
| US8025733B2 (en) | 2002-07-23 | 2011-09-27 | Samsung Mobile Display Co., Ltd. | Heating crucible and deposition apparatus using the same |
| CN101210290B (en) * | 2006-12-27 | 2012-10-10 | 通用电气公司 | Articles for use with highly reactive alloys |
| WO2012159267A1 (en) * | 2011-05-25 | 2012-11-29 | Saint-Gobain Research (Shanghai) Co., Ltd | Silica crucible and method for fabricating the same |
| CN102839350A (en) * | 2011-06-23 | 2012-12-26 | 苏州五方光电科技有限公司 | Film coater |
| CN101230424B (en) * | 2006-12-27 | 2013-09-18 | 通用电气公司 | Methods for reducing carbon contamination when melting highly reactive alloys |
| KR101505824B1 (en) * | 2006-12-22 | 2015-03-25 | 필립스 루미리즈 라이팅 캄파니 엘엘씨 | Iii-nitride light emitting devices grown on templates to reduce strain |
| CN109722551A (en) * | 2019-03-20 | 2019-05-07 | 北京欧菲金太科技有限责任公司 | The continuous producing apparatus and continuous producing method of magnesium metal |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87206316U (en) * | 1987-04-16 | 1987-12-30 | 清华大学 | Crucible with si3n4 coating |
| US5075055A (en) * | 1990-06-06 | 1991-12-24 | Union Carbide Coatings Service Technology Corporation | Process for producing a boron nitride crucible |
| CN1048751A (en) * | 1990-07-17 | 1991-01-23 | 天津大学 | Metallic crucible made of anticorrosion composite material |
-
1994
- 1994-09-10 CN CN94115523A patent/CN1039247C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8025733B2 (en) | 2002-07-23 | 2011-09-27 | Samsung Mobile Display Co., Ltd. | Heating crucible and deposition apparatus using the same |
| CN100457966C (en) * | 2002-09-03 | 2009-02-04 | 三星Sdi株式会社 | Heating crucible for organic film forming squipment |
| US7962016B2 (en) | 2002-09-03 | 2011-06-14 | Samsung Mobile Display Co., Ltd. | Heating crucible for organic thin film forming apparatus |
| KR101505824B1 (en) * | 2006-12-22 | 2015-03-25 | 필립스 루미리즈 라이팅 캄파니 엘엘씨 | Iii-nitride light emitting devices grown on templates to reduce strain |
| CN101210290B (en) * | 2006-12-27 | 2012-10-10 | 通用电气公司 | Articles for use with highly reactive alloys |
| CN101230424B (en) * | 2006-12-27 | 2013-09-18 | 通用电气公司 | Methods for reducing carbon contamination when melting highly reactive alloys |
| WO2012159267A1 (en) * | 2011-05-25 | 2012-11-29 | Saint-Gobain Research (Shanghai) Co., Ltd | Silica crucible and method for fabricating the same |
| CN102839350A (en) * | 2011-06-23 | 2012-12-26 | 苏州五方光电科技有限公司 | Film coater |
| CN109722551A (en) * | 2019-03-20 | 2019-05-07 | 北京欧菲金太科技有限责任公司 | The continuous producing apparatus and continuous producing method of magnesium metal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1039247C (en) | 1998-07-22 |
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Owner name: BEIJING STEEL INSTITUTE GAONA TECHNOLOGY LIMITED Free format text: FORMER OWNER: GENERAL RESEARCH INST. OF IRON AND STEEL, MINISTRY OF METALLURGICAL INDUSTRY Effective date: 20031211 |
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Effective date of registration: 20031211 Address after: 100081 No. 76 South College Road, Beijing Patentee after: Beijing Gaona technology limited liability company Address before: 100081 No. 76 South College Road, Beijing Patentee before: Iron and Steel Central Research Institute of Ministry of Metallurgical Industry |
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Granted publication date: 19980722 |