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 PDF

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Publication number
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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China
Prior art keywords
aliquation
hot bending
bending die
pyrolysis
coating
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CN201810480872.0A
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Inventor
刘汝强
王殿春
孙蕾
张佳伟
赵旭荣
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SHANDONG GUOJING NEW MATERIALS CO Ltd
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SHANDONG GUOJING NEW MATERIALS CO Ltd
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Priority to CN201810480872.0A priority Critical patent/CN108517511A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0254Physical 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

A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation
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.
CN201810480872.0A 2018-05-18 2018-05-18 A kind of preparation method of the hot bending die for the anti-pyrolysis equadag coating aliquation solving oxidation Pending CN108517511A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Publication number Priority date Publication date Assignee Title
JPH0788233B2 (en) * 1986-07-21 1995-09-27 東洋炭素株式会社 Graphite jig for glass molding
CN104561924A (en) * 2014-12-05 2015-04-29 林前锋 Preparation method of pyrolytic carbon coating
TW201527243A (en) * 2013-09-30 2015-07-16 Techno Quartz Inc Quartz glass component and method for producing quartz glass component
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
CN106430924A (en) * 2016-09-22 2017-02-22 凯茂科技(深圳)有限公司 Hot bending die

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104561924A (en) * 2014-12-05 2015-04-29 林前锋 Preparation method of pyrolytic carbon coating
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
CN106430924A (en) * 2016-09-22 2017-02-22 凯茂科技(深圳)有限公司 Hot bending die

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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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