CN100360707C - Production of graphite crucible for vacuum film coating - Google Patents
Production of graphite crucible for vacuum film coating Download PDFInfo
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- CN100360707C CN100360707C CNB2004100491508A CN200410049150A CN100360707C CN 100360707 C CN100360707 C CN 100360707C CN B2004100491508 A CNB2004100491508 A CN B2004100491508A CN 200410049150 A CN200410049150 A CN 200410049150A CN 100360707 C CN100360707 C CN 100360707C
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- Prior art keywords
- crucible
- plumbago crucible
- light metal
- vacuum plating
- resin
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Abstract
The present invention provides a method for making a graphite crucible for vacuum film coating, which comprises the following steps: 1), placing the graphite crucible into a dipping kettle and pumping into vacuum; 2), pumping a dipping sealant in vacuum; 3), keeping a period of time in a pressurizing state; 4), placing the graphite crucible into a curing agent which is used for curing an addition agent; 5), gradually raising temperature which does not exceed 1150 DEG C under a pressurizing condition. The dipping sealant is resin and the addition agent is also added to the resin. The addition agent is the nitrate or the sulfate of a light metal which can be dissolved into alcohol or an arbitrary proportioning mixture of the nitrate and the sulfate. The molecular weight of the light metal is below 30 and the hydroxide of the light metal is not dissolved into water and the alcohol. The curing agent is ammonium hydroxide. The method efficiently improves hole sealing effect. The graphite crucible made by the method has long service life. A circular crucible can be heated by more than 22 times and a quadrate crucible can be heated by more than 16 times.
Description
Technical field
The present invention relates to a kind of method for preparing vacuum plating with plumbago crucible.
Background technology
In vacuum aluminum-coated industry, under vacuum environment, aluminium block is placed plumbago crucible, be heated to 1600～2300 ℃, aluminium by evaporation to plastics film.This evaporation process is a kind of discontinuous operating procedure, plumbago crucible is in the heating that goes round and begins again, the cooling work state, if high temperature aluminum liquid penetrates in the plumbago crucible micropore, because the coefficient of expansion of aluminium and graphite is different, can make plumbago crucible produce the crack when reheat, aluminium liquid leaks outside and can not use from plumbago crucible.
At present, in order to address this problem, adopt the dipping sealing of hole to handle to plumbago crucible, the dipping hole sealing agent that adopts is a resene, such as resol or modified phenolic resins or Resins, epoxy etc., though this crucible improves to some extent, work-ing life is still limited, the life-span of general circular plumbago crucible is no more than 12 heating, and the life-span of square crucible is shorter.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that can prepare the vacuum plating of long service life with plumbago crucible.For this reason, the present invention is by the following technical solutions: it may further comprise the steps:
1), plumbago crucible is placed dipping still and vacuumizing,
2), suction dipping hole sealing agent under vacuum, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide
3), under pressurized state, keep for some time,
4), crucible is placed solidifying agent, with solidifying agent additive is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.
Owing to adopt above technical scheme, improved the sealing of hole effect effectively, high temperature aluminum liquid is difficult for infiltrating in the graphite, makes the pot life height that the present invention prepares, and with the crucible that this method is made, volume density is not less than 1.86g/cm
3, void content is not more than 15%, and ultimate compression strength is not less than 68.6Mpa, and resistivity is not more than 15 * 10
-4Ω cm, ash is not more than 100ppm, and circular crucible can tolerate heating more than 22 times, and square crucible can tolerate heating more than 16 times.
The present invention also can adopt following further technical scheme simultaneously:
Described light metal nitrate is the best with aluminum nitrate or sal epsom.With regard to additive, in its solubility range, should be The more the better, generally be controlled at and account for weight resin 1～15%, be good with 5～15%.
Described resene dipping hole sealing agent is the mixture of resol or modified phenolic resins or their arbitrary proportion.Certainly, other has the resin of sufficient intensity also can use after certain solubility charing is arranged in organic solvent.
The pressure range of step " 5) " is the best with 0.5Mpa～0.7Mpa.
The pressure of step " 3) " is 0.4Mpa～0.7Mpa.
Described step " 1) " vacuumize more than the 93000pa.
In addition, carrying out step " 5) " after the curing after with the crucible seasoning again.Can be convenient to make and save manufacturing cost.
All further technical schemes of the present invention are if all adopt best results simultaneously.
Embodiment
Embodiment 1
1), with ready-formed plumbago crucible (profile 210 * 100 * 60mm, interior shape 200 * 90 * 55mm, volume density 1.80g/cm
3) place dipping still and vacuumizing.Present embodiment vacuumizes more than the 93000pa.
2), suction dipping hole sealing agent under vacuum, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide.The additive of present embodiment is an aluminum nitrate, and resin is a modified phenolic resins, and aluminum nitrate accounts for 10% of resol weight, and modified phenolic resins and aluminum nitrate all are dissolved in industrial spirit earlier.
3), under pressurized state, keeping for some time, present embodiment is that 0.45Mpa kept 4 hours.
4), crucible is placed solidifying agent, with solidifying agent light metal nitrate is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.The Heating temperature of present embodiment is up to 900 ℃, and pressure is 0.6Mpa
After the curing crucible seasoning carried out again step " 5) " after 2 days.
Embodiment 2
1), with ready-formed plumbago crucible (profile Φ 135 * 120mm, interior shape Φ 120 * 110mm, volume density 1.80g/cm
3) place dipping still and vacuumizing.Present embodiment vacuumizes more than the 93000pa.
2), suction dipping hole sealing agent under vacuum, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide.The additive of present embodiment is a sal epsom, and resin is a resol, and sal epsom accounts for 12% of resol weight, and resol and aluminum nitrate all are dissolved in industrial spirit earlier.
3), under pressurized state, keeping for some time, present embodiment is that 0.55Mpa kept 5 hours.
4), crucible is placed solidifying agent, with solidifying agent light metal nitrate is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.The Heating temperature of present embodiment is up to 1000 ℃, and pressure is 0.7Mpa
After the curing crucible seasoning carried out again step " 5) " after 2 days.
Embodiment 3
1), with ready-formed plumbago crucible (profile Φ 135 * 120mm, interior shape Φ 120 * 110mm, volume density 1.80g/cm
3) place dipping still and vacuumizing.Present embodiment vacuumizes more than the 93000pa.
2), at the dipping of suction under vacuum hole sealing agent, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide.The additive of present embodiment is the mixture of aluminum nitrate and sal epsom each half, resin is resol and 8: 2 by weight percentage mixture of modified phenolic resins, aluminum nitrate and sal epsom mixture account for 8% of resin compound weight, and resin and additive all are dissolved in industrial spirit earlier.
3), keep for some time under pressurized state, present embodiment is that 0.65Mpa kept 5 hours.
4), crucible is placed solidifying agent, with solidifying agent light metal nitrate is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.The Heating temperature of present embodiment is up to 1050 ℃, and pressure is 0.5Mpa
Before curing,, under the 0.4Mpa pressured state, kept 6 hours crucible scraping surface.After the curing crucible seasoning carried out again step " 5) " after 2 days.
Embodiment 4
1), with ready-formed plumbago crucible (profile 210 * 100 * 60mm, interior shape 200 * 90 * 55mm, volume density 1.80g/cm
3) place dipping still and vacuumizing.The vacuum tightness of present embodiment is more than the 93000pa,
2), suction dipping hole sealing agent under vacuum, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide.The additive of present embodiment is aluminum nitrate and 3: 7 by weight percentage mixture of sal epsom, resin is the mixture of resol and modified phenolic resins each half, aluminum nitrate and sal epsom mixture account for 3% of resin compound weight, and resin and additive all are dissolved in industrial spirit earlier.
3), keep for some time under pressurized state, present embodiment is that 0.65Mpa kept 5 hours.
4), crucible is placed solidifying agent, with solidifying agent light metal nitrate is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.The Heating temperature of present embodiment is up to 1050 ℃, and pressure is 0.5Mpa
After the curing crucible seasoning carried out again step " 5) " after 2 days.
Following table is the index summary sheet of the prepared crucible of each embodiment.
| Performance | Work-ing life (number of times) | |||||
| Volume density (g/cm 3) | Void content is not more than (%) | Ultimate compression strength is not less than (Mpa) | Resistivity is not more than (* 10 -4Ω cm) | Ash is not more than (ppm) | ||
| Embodiment 1 | ?1.86 | ?15 | ?68.6 | ?15 | ?100 | ＞16 |
| Embodiment 2 | ?1.86 | ?15 | ?68.6 | ?15 | ?100 | ＞22 |
| Embodiment 3 | ?1.86 | ?15 | ?68.6 | ?15 | ?100 | ＞22 |
| Embodiment 4 | ?1.86 | ?15 | ?68.6 | ?15 | ?100 | ＞16 |
Claims (9)
1, a kind of method for preparing vacuum plating with plumbago crucible is characterized in that it may further comprise the steps:
1), plumbago crucible is placed dipping still and vacuumizing,
2), suction dipping hole sealing agent under vacuum, the dipping hole sealing agent that is adopted is a resin, also be added with additive in the resin, described additive is for being dissolved in light metal nitrate or the vitriol or their the arbitrary proportion mixture of alcohol, light metal is a molecular weight less than 30 metal, and the water insoluble and alcohol of its oxyhydroxide
3), the pressurization,
4), crucible is placed solidifying agent, with solidifying agent additive is cured, solidifying agent is an ammoniacal liquor,
5), progressively heat up under the condition of pressurization, top temperature is no more than 1150 ℃.
2, a kind of method for preparing vacuum plating with plumbago crucible as claimed in claim 1 is characterized in that described light metal nitrate is aluminum nitrate, and light metal vitriol is sal epsom.
3, a kind of method for preparing vacuum plating with plumbago crucible as claimed in claim 1 is characterized in that described additive accounts for weight resin 1～15%.
4, a kind of method for preparing vacuum plating with plumbago crucible as claimed in claim 1 is characterized in that described additive accounts for weight resin 5～15%.
5, as claimed in claim 1ly a kind ofly prepare vacuum plating with the method for plumbago crucible, it is characterized in that the pressure range of step " 5) " is 0.5Mpa～0.7Mpa.
6, a kind of method for preparing vacuum plating with plumbago crucible as claimed in claim 1 is characterized in that described resene dipping hole sealing agent is the mixture of resol or modified phenolic resins or their arbitrary proportion.
7, as claimed in claim 1ly a kind ofly prepare vacuum plating with the method for plumbago crucible, it is characterized in that described step " 1) " vacuumizes more than the 93000pa.
8, describedly a kind ofly prepare vacuum plating with the method for plumbago crucible as weighing 1, it is characterized in that the pressure of step " 3) " is 0.4Mpa～0.7Mpa.
9, describedly a kind ofly prepare vacuum plating with the methods of plumbago crucible as weighing 1,2,3,4,5,6,7 or 8, it is characterized in that carrying out step " 5) " after the curing after with the crucible seasoning again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100491508A CN100360707C (en) | 2004-06-22 | 2004-06-22 | Production of graphite crucible for vacuum film coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100491508A CN100360707C (en) | 2004-06-22 | 2004-06-22 | Production of graphite crucible for vacuum film coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1712555A CN1712555A (en) | 2005-12-28 |
| CN100360707C true CN100360707C (en) | 2008-01-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100491508A Expired - Fee Related CN100360707C (en) | 2004-06-22 | 2004-06-22 | Production of graphite crucible for vacuum film coating |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441842A (en) * | 2018-05-24 | 2018-08-24 | 山东伟基炭科技有限公司 | A kind of band antioxidant coating tubular type PECVD graphite boats and manufacturing method |
| CN110699628A (en) * | 2019-10-14 | 2020-01-17 | 洛阳轴承研究所有限公司 | Hole sealing method of plasma spraying coating and insulating bearing |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062178A (en) * | 1990-11-29 | 1992-06-24 | 中国科学院计算技术研究所 | The adhering method of cathode target of vacuum sputter system |
| US20040086717A1 (en) * | 2002-06-14 | 2004-05-06 | Avery Dennison Corporation | Transparent conductive film for flat panel displays |
-
2004
- 2004-06-22 CN CNB2004100491508A patent/CN100360707C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062178A (en) * | 1990-11-29 | 1992-06-24 | 中国科学院计算技术研究所 | The adhering method of cathode target of vacuum sputter system |
| US20040086717A1 (en) * | 2002-06-14 | 2004-05-06 | Avery Dennison Corporation | Transparent conductive film for flat panel displays |
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| Publication number | Publication date |
|---|---|
| CN1712555A (en) | 2005-12-28 |
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Granted publication date: 20080109 Termination date: 20130622 |