CN1039247C - Crucible with titanium diboride coating and its manufacture - Google Patents
Crucible with titanium diboride coating and its manufacture Download PDFInfo
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- CN1039247C CN1039247C CN94115523A CN94115523A CN1039247C CN 1039247 C CN1039247 C CN 1039247C CN 94115523 A CN94115523 A CN 94115523A CN 94115523 A CN94115523 A CN 94115523A CN 1039247 C CN1039247 C CN 1039247C
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- crucible
- coated
- titanium diboride
- groove
- diboride coating
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Abstract
The present invention provides a crucible with a titanium diboride coating, which relates to a vacuum coating crucible or a filming crucible for smelting metal. The crucible has a crucible body with a groove, and the inner wall of the groove of the crucible is coated with a titanium diboride coating. The surface part of the upper wall of the crucible or all the crucible is coated with an aluminium oxide or silicon dioxide insulation protecting layer. The crucible has the advantages of electric conduction, enhancement of molten metal corrosion resistance, long service life, etc. and also discloses a method for manufacturing the crucible with a titanium diboride coating.
Description
The present invention relates to a kind of improved crucible, particularly a kind of vacuum coat 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 unit, 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 compound, 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 compound wherein and nitride mostly are electrically nonconducting material or insulating material, 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.
One of the present invention provides 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 aluminium sesquioxide 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 aluminium sesquioxide 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 compound, though nitride crucible or its composite crucible can overcome above-mentioned deficiency, but its poorly conductive, be unsuitable for doing the electrode crucible, and select for use TiB2 to make crucible coating layer, its reason is that TiB2 has the fusing point height, reaches 2930 ℃, conduct electricity very well, ρ room temperature=12 μ ncm, and advantage such as chemical stability is good, and wear resistance is strong, the refractory metal crucible that scribbles TiB2 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 and produce reaction between the metal of crucible and institute deposite metal, alloying or fusion, and as copper crucible, need need not water-cooled.
Top wall surface at crucible scribbles insulating protective layers such as aluminium sesquioxide or silicon-dioxide, 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) TiB2 is coated on the inwall of described crucible groove, until being coated on till TiB2 on the crucible groove inwall reaches desired thickness;
(c) aluminium sesquioxide or silicon-dioxide partly or entirely are coated on the top wall surface of described crucible, till the aluminium sesquioxide that is coated on the crucible top wall surface or silicon-dioxide reach desired thickness.
Here to be coated on the desired thickness of titanium diboride coating on the described crucible groove inwall be 0.2～2mm to indication.
The aluminium sesquioxide or the desired thickness of silicon-dioxide that are coated 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 aggressiveness is good, because crucible of the present invention adopts TiB2 to make the groove inside coating, the TiB2 fusing point is up to 2930 ℃, and chemical stability is good, wear resistance 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, therefore electricalresistivity's room temperature of TiB2=12 μ ncm is body with the refractory metal, is that the crucible of coating has good electrical conductivity with the TiB2.
(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, foreign matter content is low, and crucible can use tens times to tens times.
The 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 Resins, epoxy with titanium diboride powder furnishing pasty state, the weight ratio of Resins, epoxy and TiB2 is 0.1～1;
(3) crucible groove inwall is sprayed noisy, cleaning, make its inwall for there not being oily, dustless hair side;
(4) the pasty state TiB2 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 organism volatilization, be warming up to 1300 ℃ of sintering then 1～4 hour;
(6) top wall surface at crucible partly or entirely applies aluminium sesquioxide or silica slurry, and its thickness is as required: 0.1～1.0mm;
(7) treat aluminium sesquioxide or silica slurry seasoning 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 aluminium sesquioxide 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
| Form lot number | The crucible bulk material | Titanium diboride coating thickness (mm) | Aluminum oxide coating thickness (mm) | Silica dioxide coating thickness (mm) |
| 1 | Tungsten | 0.3 | ?0.2 | / |
| 2 | Molybdenum | 1.0 | ?0.8 | / |
| 3 | Tantalum | 1.8 | / | 0.9 |
The performance of table 2 embodiment crucible
| The performance lot number | The electroconductibility of crucible (1) | Insulation layer insulativity (2) | Crucible life (3) |
| 1 | ＜1Ω | ＞10MΩ | 15 times |
| 2 | ＜1Ω | ＞20MΩ | 22 times |
| 3 | ＜1Ω | ＞2MΩ | 24 times |
Annotate (1) electroconductibility with volt ohm-milliammeter 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 insulation layer insulativity method is the same, and just black meter pen slides on insulation layer.
(3) work-ing life of crucible, can be regarded as once with vacuum arc evaporation 10 gram nickel.
Claims (2)
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; thickness is 0.2-2mm; top wall surface at described crucible body partly or entirely is coated with aluminium sesquioxide or silicon dioxide insulator protective layer, and thickness is: 0.1-1.0mm.
2, 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) TiB2 is coated on the inwall of described crucible groove, until being coated on till TiB2 on the crucible groove inwall reaches 0.2-2mm;
(c) aluminium sesquioxide or silicon-dioxide partly or entirely are coated on the top wall surface of described crucible, till the aluminium sesquioxide that is coated on the crucible top wall surface or silicon-dioxide reach 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 CN1104758A (en) | 1995-07-05 |
| CN1039247C true 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) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100490537B1 (en) | 2002-07-23 | 2005-05-17 | 삼성에스디아이 주식회사 | Heating crucible and deposit apparatus utilizing the same |
| KR100889758B1 (en) | 2002-09-03 | 2009-03-20 | 삼성모바일디스플레이주식회사 | Heating crucible of organic thin film forming apparatus |
| US7547908B2 (en) * | 2006-12-22 | 2009-06-16 | Philips Lumilieds Lighting Co, Llc | III-nitride light emitting devices grown on templates to reduce strain |
| US7790101B2 (en) * | 2006-12-27 | 2010-09-07 | General Electric Company | Articles for use with highly reactive alloys |
| US7582133B2 (en) * | 2006-12-27 | 2009-09-01 | General Electric Company | Methods for reducing carbon contamination when melting highly reactive alloys |
| EP2616575A4 (en) * | 2011-05-25 | 2015-05-20 | Saint Gobain Res 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 |
Citations (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 |
| CN1048751A (en) * | 1990-07-17 | 1991-01-23 | 天津大学 | Metallic crucible made of anticorrosion composite material |
| CN1058091A (en) * | 1990-06-06 | 1992-01-22 | 联合碳化涂料服务技术公司 | Borium nitride crucible and manufacture method thereof |
-
1994
- 1994-09-10 CN CN94115523A patent/CN1039247C/en not_active Expired - Fee Related
Patent Citations (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 |
| CN1058091A (en) * | 1990-06-06 | 1992-01-22 | 联合碳化涂料服务技术公司 | Borium nitride crucible and manufacture method thereof |
| CN1048751A (en) * | 1990-07-17 | 1991-01-23 | 天津大学 | Metallic crucible made of anticorrosion composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1104758A (en) | 1995-07-05 |
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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 |