CN108517511A - A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation - Google Patents
A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation Download PDFInfo
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- CN108517511A CN108517511A CN201810480872.0A CN201810480872A CN108517511A CN 108517511 A CN108517511 A CN 108517511A CN 201810480872 A CN201810480872 A CN 201810480872A CN 108517511 A CN108517511 A CN 108517511A
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- Prior art keywords
- aliquation
- hot bending
- bending die
- pyrolysis
- coating
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing
Abstract
The present invention relates to a kind of preparation methods of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation, the method of the present invention by strictly controlling hot bending die Substrate Surface Roughness, specific warming temperature, pressure, specific cooling hasten, matrix tolerance and anti-aliquation slot, overall coordination improves the binding force of coating and matrix, avoid product rejection problem caused by product aliquation, the yields of product promotes 23 times, the service life of product promotes 45 times, and corresponding cost also reduces by 60% or more.
Description
Technical field
The present invention relates to a kind of preparation methods of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation, belong to heat
Bending mould technical field.
Background technology
With the progress of industrial level and the increasingly raising of living standards of the people, single plate glass has been unable to meet people
Demand, pattern is beautiful, the lines flow smoothly, the heat-bending glass of using flexible is also more and more in building, the use of civilian occasion.
Currently, the mold used in compacting 3D mobile phone glass, is generally made of a punch-pin and a cavity plate.In the machine-shaping of glass
The periphery of Cheng Zhong, glass generate bending by heating and ambient pressure.
Hot bending die at present it is most commonly used be pure graphite material hot bending die, due to graphite material hole it is more, it is oxidizable,
The shortcomings that discharging gas in generation impurity and production process, Many researchers are being tested at present applies one layer of guarantor on graphite
Sheath makes up the shortcoming of pure graphite material itself.Coating mostly carries out depositing to graphite using chemical vapor deposition method
Die surface.
By deposit pyrolytic graphite coating by graphite matrix package can be very good solve problem of oxidation, isolation graphite it is miscellaneous
Matter, in deposition after pyrolytic graphite coating, during practical later stage use, due to hot bending die structure, the particularity of shape, heat
The corner angle of bending mould structure are more, and unlike crucible die, pyrolytic graphite coating has been easy side, blistering, cracking, causes pyrolytic graphite
The different degrees of aliquation of coating even falls off when serious, the qualification rate, service life and quality of hot bending die is caused to drop significantly
It is low.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation side of the hot bending die of anti-pyrolysis equadag coating aliquation
Method.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation, including step:
(1) graphite material hot bending die matrix carves anti-aliquation slot, coarse processing, hot bending die matrix surface after coarse processing
Roughness is:0.1-6.4 microns;
(2) coarse treated that hot bending die matrix is hanging in reacting furnace, closes bell, vacuumizes heating, and heating is warm
Degree control is at 1700~2300 DEG C, and reaction furnace pressure control is in 30-500Pa;
(3) under inert gas protection, it is passed into alkanes as reaction gas in reacting furnace, makes hot bending die matrix table
Last layer pyrolytic graphite coating is deposited with the deposition velocity of micro- m/h of 5-30 on face;
(4) when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches 10-100 (5-150) micron, stop
It is passed through gas, reacting furnace Temperature fall 24-48 hours;
(5) after being naturally cooling to room temperature, the hot bending die of anti-pyrolysis equadag coating aliquation is obtained.
According to currently preferred, hot bending die Substrate Surface Roughness is after coarse processing:0.5-3.2 microns;It is preferred that
, hot bending die Substrate Surface Roughness is after coarse processing:1.0-2.0 micron.
Due to hot bending die structure, the particularity of shape, the corner angle of hot bending die structure are more, used after depositing coating
Easily aliquation, the present invention should strictly control hot bending die Substrate Surface Roughness, hot bending die Substrate Surface Roughness mistake in journey
The big or too small binding force that can influence coating and matrix causes coating aliquation, control hot bending die Substrate Surface Roughness to be
Present inventor gives a lesson to pleasantly surprised discovery by failure experience many times, and control hot bending die Substrate Surface Roughness can be right
Hot bending die coating aliquation has conclusive influence, and the roughness is unlike other surfaces processing, and the factor of consideration is different, the present invention
The control of roughness need to consider many factors such as special structure, shape and the aliquation of hot bending die.
According to currently preferred, hot bending die matrix includes lower die for placing glass and for depressing glass
Mould is adapted to connection between the lower die and upper mold.
According to currently preferred, the tolerance of hot bending die matrix is 0.005-0.02mm.
According to currently preferred, anti-aliquation groove depth is 0.5-3mm on graphite material hot bending die matrix, under being located at
The non-working surface of mould, upper mold.
Anti- aliquation slot is rectangular recess, and width 5-20mm, length is to prolong on one side from mold on die width direction
Another side is extended to, anti-aliquation slot is dip-parallel to be arranged in the back side of lower die, upper mold, the distance between anti-aliquation slot and anti-aliquation slot
For 20-100mm.
It is further preferred that the distance between anti-aliquation slot and anti-aliquation slot are 20-30mm.
The anti-aliquation slot of present invention pyrolytic graphite coating in gradually scatter coated to graphite material hot bending die matrix
Stress inside coating material, while playing the role of enhancing binding force, so that coating is bonded with matrix even closer, protects simultaneously
Demonstrate,prove the robustness of mold.
According to currently preferred, step (2) is coarse, and treated that hot bending die matrix is hanging in reacting furnace vertically, sinks
When product, spacing distance is more than or equal to 5mm between hot bending die matrix.
The advantages of such design:Shadow of the modes of emplacement of coarse treated the hot bending die matrix of the present invention by terrestrial gravitation
Sound can ensure that each corner coating on hot bending die matrix of pyrolytic graphite coating is uniform, while avoid mutual shadow between product
Ring the unevenness for causing thickness distribution.
According to currently preferred, in step (2), the gas in stove is uniformly distributed that region, that temperature is uniformly distributed region is big
In the height equal to hot bending die matrix.
According to currently preferred, in step (2), warming temperature is controlled at 1800-2100 DEG C;Preferably, warming temperature
Control is at 1900-2000 DEG C.Due to hot bending die structure, the particularity of shape, deposition pyrolytic graphite coating controls depositing temperature,
It can be crystallized to avoid coat inside and more be intended to unanimously, make coat inside crystallization consistency weaken, make the pyrolysis stone of deposition
Black coating is neither too hard, nor too soft, and coating is avoided to be hardened, coating cracking and layering when preventing from cooling down.
According to currently preferred, in step (2), reaction furnace pressure control is in 100-300Pa;Preferably, reacting furnace
Interior pressure control is in 200-300Pa.
The alkanes reaction gas of the present invention is methane, and methane is slow relative to the reaction gas reaction rate such as ethane and propane,
Easily controllable, the thickness difference of Bulk coat can control within 5 microns.
According to currently preferred, in step (3), the deposition velocity control of pyrolytic graphite coating 10-15 microns/it is small
When.
The deposition velocity of the present invention can reduce the stress in pyrolytic graphite layer and improve pyrolytic graphite inter-layer bonding force, make
Layer internal stress is released, and so that inter-layer bonding force is enhanced, coat inside is avoided to be layered.
The cooling of the present invention hastens to be maintained at Temperature fall 24-48 hours, avoids cooling down too fast, coating is hardened, and prevents from dropping
Coating cracking and layering when warm.
According to currently preferred, in step (4), when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches
Stop being passed through gas at 10-60 microns.
Beneficial effects of the present invention are:
1, method of the invention by strictly control hot bending die Substrate Surface Roughness, specific warming temperature, pressure,
Specific cooling hastens, matrix tolerance and anti-aliquation slot, overall coordination improve the binding force of coating and matrix, avoids production
The yields of product rejection problem caused by product aliquation, product promotes 2-3 times, and the service life of product promotes 4-5 times, accordingly
Cost also reduce by 60% or more.
Description of the drawings
Fig. 1 is the hot bending die structural schematic diagram of anti-pyrolysis equadag coating aliquation produced by the present invention;
Wherein, 1, anti-aliquation slot, 2, circular arc chamfering.
Specific implementation mode
The present invention is further limited with embodiment with reference to the accompanying drawings of the specification, but not limited to this.
Embodiment 1
A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation, including step:
(1) margin of tolerance of graphite material hot bending die matrix is 0.01-0.02mm, in hot bending die lower die, upper mold
Anti- aliquation slot is carved at the back side respectively, and anti-aliquation slot is rectangular recess, and length is to extend on one side from mold on die width direction
To another side, anti-aliquation groove depth is 1.2mm, width 10mm, then coarse processing is carried out to die matrix, after coarse processing
Hot bending die Substrate Surface Roughness is:1.6 micron;
(2) coarse treated that hot bending die matrix is hanging in reacting furnace vertically, interval distance between hot bending die matrix
From for 60mm, gas distribution regions, Temperature Distribution region in stove are more than or equal to the height of hot bending die matrix, close bell,
Heating is vacuumized, warming temperature is controlled at 2000 DEG C, and reaction furnace pressure control is in 300PaPa;
(3) under protection of argon gas, be passed into methane as reaction gas in reacting furnace, make on hot bending die matrix surface with
5 micro- ms/h of deposition velocity deposits last layer pyrolytic graphite coating;
(4) when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches 40 microns, stopping is passed through gas, instead
Answer stove Temperature fall 24-48 hours;
(5) after being naturally cooling to room temperature, the hot bending die of anti-pyrolysis equadag coating aliquation is obtained.
Embodiment 2
A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation, including step:
(1) margin of tolerance of graphite material hot bending die matrix is 0.01-0.02mm, in hot bending die lower die, upper mold
Anti- aliquation slot is carved at the back side respectively, and anti-aliquation slot is rectangular recess, and length is to extend on one side from mold on die width direction
To another side, anti-aliquation groove depth is 2.6mm, width 15mm, then coarse processing is carried out to die matrix, after coarse processing
Hot bending die Substrate Surface Roughness is:1 micron;
(2) coarse treated that hot bending die matrix is hanging in reacting furnace vertically, interval distance between hot bending die matrix
From for 60mm, gas distribution regions, Temperature Distribution region in stove are more than or equal to the height of hot bending die matrix, close bell,
Heating vacuumizes, and warming temperature is controlled at 2200 DEG C, and reaction furnace pressure control is in 200Pa;
(3) under protection of argon gas, be passed into methane as reaction gas in reacting furnace, make on hot bending die matrix surface with
10 micro- ms/h of deposition velocity deposits last layer pyrolytic graphite coating;
(4) when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches 40 microns, stopping is passed through gas, instead
Answer stove Temperature fall 24-48 hours;
(5) after being naturally cooling to room temperature, the hot bending die of anti-pyrolysis equadag coating aliquation is obtained.
Embodiment 3
With the preparation method of the hot bending die of the anti-pyrolysis equadag coating aliquation of embodiment 1, the difference is that:
The anti-aliquation groove depth of step (1) be 0.6mm, width 20mm,
Influence of the 1 anti-aliquation groove depth of experimental example to coating
Carry out preparing the pyrolytic graphite coating hot bending die of anti-aliquation as described in Example 1, the difference is that, change
The depth of anti-aliquation slot, respectively 0.1mm, 0.3mm, 4mm, 5mm, 7mm, 8mm, 10mm, obtained pyrolytic graphite coating hot bending
Mold, which puts into production, to be compared, and as a result see the table below 1:
Table 1
Anti- aliquation groove depth | Coating aliquation situation |
0.1mm | Complete aliquation is not used in product |
0.3mm | 1/2 area aliquation is not used in product |
Embodiment 1 | Using at 1000 times, no cracking, aliquation |
4mm | Using at 800 times, notch cracking, surface is without aliquation |
5mm | Using at 600 times, notch cracking, surface is without aliquation |
7mm | Using at 200 times, notch cracks, surface aliquation |
8mm | Notch cracking, aliquation is not used in product |
10mm | Complete aliquation is not used in product |
Influence of the 2 anti-aliquation well width of experimental example to coating
Carry out preparing the pyrolytic graphite coating hot bending die of anti-aliquation as described in Example 1, the difference is that, change
The width of anti-aliquation slot, respectively 4mm, 8mm, 25mm, 28mm, 30mm, 35mm, 40mm, obtained pyrolytic graphite coating hot bending
Mold, which puts into production, to be compared, and as a result see the table below 1:
Table 1
The width of anti-aliquation slot | Coating aliquation situation |
4mm | Complete aliquation is not used in product |
8mm | Notch aliquation is not used in product |
Embodiment 1 | Using at 1000 times, no cracking, aliquation |
25mm | Using at 800 times, notch is crack to be split |
28mm | Using at 700 times, notch is crack to be split |
30mm | Using at 200 times, notch serious cracking |
35mm | Notch aliquation is not used in product |
40mm | Complete aliquation is not used in product |
3 reaction temperature of experimental example is to the hardness of production process floating coat and the influence of aliquation
Carry out preparing the pyrolytic graphite coating hot bending die of anti-aliquation as described in Example 1, the difference is that, change
Warming temperature, warming temperature are controlled respectively at 1500 DEG C, 1600 DEG C, 2300 DEG C, 2400 DEG C, obtained pyrolytic graphite coating hot bending
Mold, which puts into production, to be compared, and as a result see the table below 2:
Table 2
Warming temperature | Deposition process floating coat hardness | Aliquation situation |
1500℃ | It is soft | Without aliquation, cannot produce and use |
1600℃ | It is softer | Without aliquation, post-processing requirement is not achieved |
Embodiment 1 | It is neither too hard, nor too soft | Using at 1000 times, no cracking, aliquation |
2300℃ | It is harder | Using at 500 times, product cracking, aliquation |
2400℃ | Firmly | All crackings have been not used in product |
4 deposition velocity of experimental example is to the hardness of production process floating coat and the influence of aliquation
Carry out preparing the pyrolytic graphite coating hot bending die of anti-aliquation as described in Example 1, the difference is that, change
Deposition velocity, deposition velocity are respectively 1 micro- m/h, 3 micro- ms/h, 35 micro- ms/h, 40 micro- ms/h, 50 microns/
Hour, obtained pyrolytic graphite coating hot bending die, which puts into production, to be compared, and as a result see the table below 4:
Table 4
Deposition velocity | Deposition process floating coat hardness | Aliquation situation |
1 micro- m/h | Firmly | Whole aliquations are not used in product |
3 micro- ms/h | It is harder | Using at 10 times be aliquation |
Embodiment 1 | It is neither too hard, nor too soft | Using at 1000 times, no cracking, aliquation |
35 micro- ms/h | It is softer | Using at 800 times, no cracking, aliquation |
40 micro- ms/h | It is softer | Using at 500 times, the micro- aliquation in surface |
50 micro- ms/h | It is soft | 2/3 area aliquation is not used in product |
Claims (10)
1. a kind of preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation, including step:
(1) graphite material hot bending die matrix carves anti-aliquation slot, coarse processing, and hot bending die matrix surface is coarse after coarse processing
Degree is:0.1-6.4 microns;
(2) coarse treated that hot bending die matrix is hanging in reacting furnace, closes bell, vacuumizes heating, warming temperature control
System is at 1700~2300 DEG C, and reaction furnace pressure control is in 30-500Pa;
(3) under inert gas protection, it is passed into reacting furnace, makes on hot bending die matrix surface using alkanes as reaction gas
Last layer pyrolytic graphite coating is deposited with micro- m/h of deposition velocities of 5-30;
(4) when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches 10-100 (5-150) micron, stop being passed through
Gas, reacting furnace Temperature fall 24-48 hours;
(5) after being naturally cooling to room temperature, the hot bending die of anti-pyrolysis equadag coating aliquation is obtained.
2. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that step
Suddenly hot bending die Substrate Surface Roughness is after coarse processing in (1):0.5-3.2 microns;Preferably, hot bending mould after coarse processing
Having Substrate Surface Roughness is:1.0-2.0 micron.
3. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that heat
Bending mould matrix includes the lower die for placing glass and the upper mold for depressing glass, the company of adaptation between the lower die and upper mold
It connects;The tolerance of hot bending die matrix is 0.005-0.02mm.
4. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that stone
Anti- aliquation groove depth is 0.5-3mm on black material hot bending die matrix, is located at the non-working surface of lower die, upper mold;Anti- aliquation slot is
Rectangular recess, width 5-20mm, length are to extend to another side, anti-aliquation slot on one side from mold on die width direction
Dip-parallel to be arranged at the back side of lower die, upper mold, the distance between anti-aliquation slot and anti-aliquation slot are 20-100mm.
5. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 4, which is characterized in that anti-
The distance between aliquation slot and anti-aliquation slot are 20-30mm.
6. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that step
Suddenly (2) it is coarse treated that hot bending die matrix is hanging in reacting furnace vertically, when deposition, interval distance between hot bending die matrix
From more than or equal to 5mm.Gas in stove is uniformly distributed region, temperature is uniformly distributed the height that region is more than or equal to hot bending die matrix
Degree.
7. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that step
Suddenly in (2), warming temperature is controlled at 1800-2100 DEG C;Preferably, warming temperature control is at 1900-2000 DEG C.
8. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that step
Suddenly in (2), reaction furnace pressure control is in 100-300Pa;Preferably, the control of reaction furnace pressure is in 200-300Pa.
9. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that institute
The alkanes reaction gas stated is methane, and in step (3), the deposition velocity control of pyrolytic graphite coating is in micro- m/h of 10-15.
10. the preparation method of the hot bending die of anti-pyrolysis equadag coating aliquation according to claim 1, which is characterized in that
In step (4), stop being passed through gas when the thickness of pyrolytic graphite coating on hot bending die matrix surface reaches 10-60 microns.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110016652A (en) * | 2019-04-12 | 2019-07-16 | 山东国晶新材料有限公司 | It is a kind of for making the preparation method and applications of the pyrolytic boron nitride plate of supporting rod |
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CN105483642A (en) * | 2016-01-22 | 2016-04-13 | 山东国晶新材料有限公司 | Preparation method of PBN (pyrolytic boron nitride) crucible mold with long service life |
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JPH0788233B2 (en) * | 1986-07-21 | 1995-09-27 | 東洋炭素株式会社 | Graphite jig for glass molding |
TW201527243A (en) * | 2013-09-30 | 2015-07-16 | Techno Quartz Inc | Quartz glass component and method for producing quartz glass component |
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CN110016652B (en) * | 2019-04-12 | 2020-04-24 | 山东国晶新材料有限公司 | Preparation method of pyrolytic boron nitride plate for manufacturing clamping rod |
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