CN104926311A - Reaction sintering silicon carbide ceramic uniform-temperature plate - Google Patents
Reaction sintering silicon carbide ceramic uniform-temperature plate Download PDFInfo
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- CN104926311A CN104926311A CN201510334220.2A CN201510334220A CN104926311A CN 104926311 A CN104926311 A CN 104926311A CN 201510334220 A CN201510334220 A CN 201510334220A CN 104926311 A CN104926311 A CN 104926311A
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- carbide ceramic
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Abstract
The invention discloses a reaction sintering silicon carbide ceramic uniform-temperature plate. A manufacturing method of the reaction sintering silicon carbide ceramic uniform-temperature plate comprises the steps that powder is prepared, wherein carbon and silicon carbide are mixed and added with zinc stearate and polyvinyl alcohol for spray granulation, and powder is prepared; briquettes are pressed; vacuum sintering is carried out, and silica powder is placed on the surface of the briquettes for reaction sintering; oxidation sintering is carried out, wherein oxidation sintering is carried out on the obtained uniform-temperature plate. The manufacturing method is applicable to manufacturing uniform-temperature plates of different thicknesses, appearances and structures, and the plate is compact in texture, accurate in size and high in yield. The reaction sintering silicon carbide ceramic uniform-temperature plate is good in heat conduction performance, high in high-temperature strength, low in thermal expansion coefficient and good in high-temperature corrosion resistance; particularly, the siliconing reaction is more sufficient through sintering at temperature of 1800-1900 DEG C exceeding normal reaction temperature, the texture compactness is ensured, and product cracking is avoided; in addition, by means of high-temperature oxidation sintering, the stress changes of the product at high temperature can be detected, the quality problem is prevented from being caused in the application process, and the application cost is lowered.
Description
Technical field
The present invention relates to a kind of reaction sintering silicon carbide ceramic temperature-uniforming plate, is the critical material that liquid crystal glass base produces in (TFT-LCD) molding procedure major process unit.
Background technology
TFT-LCD(liquid crystal panel) advantage such as to have volume little, lightweight, Low emissivity, less energy-consumption, true color, kinds of displays material is widely used.And glass substrate is the core component of TFT-LCD and important substance basis, it is the extremely smooth thin glass sheet in a kind of surface.Substantially, a slice TFT-LCD need use two sheet glass substrates, and the base plate being made for bottom glass substrate and colored filter (COLOR FILTER) respectively uses.The production method of glass substrate has 3 kinds: float glass process, overflow downdraw, slot draw method, its industry occupies critical role in whole liquid crystal panel industrial chain, and a lot of Performance Ratios of liquid-crystal display are as all closely related with the performance of glass substrate in resolving power, transparence, weight, visual angle etc.
The liquid crystal glass base of press over system manufacture is without the need to carrying out surface grinding processing, and quality is good, and manufacturing cost is lower, becomes the main stream approach that current liquid crystal glass base manufactures.Wherein, samming sheet material in molding procedure major process unit, its heat-conductive characteristic and high-temperature corrosion-resistance performance are not good, hot strength is low, thermal expansivity is high, when equipment well heater heats with a type of heating, easily make glass-board surface be heated irregular, be difficult to control shaping glass sheets thickness.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of reaction sintering silicon carbide ceramic temperature-uniforming plate and preparation method thereof, it has good heat conductivility and high-temperature behavior, can play critical effect to raising glass substrate quality.
To achieve these goals, the present invention adopts following technical scheme.
A kind of reaction sintering silicon carbide ceramic temperature-uniforming plate, its manufacture method comprises the following steps:
Prepare powder: by carbon with silicon carbide by 1:(2 ~ 5) mass ratio mix after, add the Zinic stearas of total mass 1% ~ 4% as lubricant, the polyvinyl alcohol of total mass 15% ~ 25% is as caking agent, and mist projection granulating, obtains powder;
Compacting briquet;
Vacuum sintering: the silica flour placing relative briquet weight 30 ~ 40% on briquet surface, carries out reaction sintering; Within 28 ~ 36h time period, vacuumize intensification and be heated to 1800 ~ 1900 DEG C, through siliconising, constant temperature, then fill helium and be cooled to 1100 ~ 1200 DEG C, then inflated with nitrogen cools to less than 120 DEG C;
Oxidation and sinter: the temperature-uniforming plate obtained is carried out oxidation and sinter; Within 200 ~ 250h time period, be slowly warming up to 1100 ~ 1200 DEG C, constant temperature 24h, then below slow cooling to 120 DEG C.
As a further improvement on the present invention, describedly prepare in the step of powder, the water content of the powder obtained is 2 ~ 5%.
The mass ratio of described carbon and silicon carbide is 1:4.
The add-on of described lubricant is 2% of total mass.
The add-on of described caking agent is 20% of total mass.
Further, the step of biscuit machine-shaping is also comprised after the step of described compacting briquet.
Also comprise the step of finishing after the step of described biscuit machine-shaping, the object of finishing is the surface imperfection eliminating biscuit.
Also comprise the step of oven dry after the step of described finishing, specifically comprise: the cryodrying carrying out temperature 60 ~ 70 DEG C, time 24 ~ 48h, then carry out temperature 80 ~ 100 DEG C, the time is the high temperature drying of 12 ~ 24h.
Also comprise the step of impurity cleaning after the step of described vacuum sintering, impurity cleaning is to accompany impurity such as burning thing to remove to the remnants on each surface of finished product of coming out of the stove.
The step of attrition process is also comprised: reach physical dimension tolerance≤± 0.5mm after attrition process, upper and lower surfaceness≤6.3 μm after the step of described impurity cleaning.
Silicon carbide ceramics has that hot strength is large, oxidation-resistance is strong, Heat stability is good, thermal expansivity are little, thermal conductivity is large, hardness is high, wear-resistant and anti-thermal shock and the good characteristic such as corrosion-resistant, be widely used in the industrial circle under the rigor condition such as high temperature, high pressure, burn into radiation, wearing and tearing, as mechanical sealing member, high-temperature heat exchanger, pyroceramic radiant burner, the long-lived kiln furnitures of high-load etc., be also considered to manufacture the most promising candidate material of internal combustion turbine, rocket nozzle and engine parts in universe and automotive industry.
All advantages of silicon carbide ceramics have been acted on silicon carbide reaction-sintered prepared by reaction sintering technology, comprise: intensity is high, hardness is high, good thermal shock, wear resistance and good corrosion resistance, thermal conductivity is high, the coefficient of expansion is low and excellent antioxidant property, and void content is low, it is a kind of Hi-tech ceramic material of excellent performance.
The invention has the beneficial effects as follows, be suitable for the making of different thickness temperature-uniforming plate contour structures form, dense materials, size are accurate, yield rate is high.The temperature-uniforming plate that the present invention makes has good heat-conductive characteristic, higher hot strength and low thermal coefficient of expansion, and good high-temperature corrosion-resistance performance, the point type of heating of equipment well heater can be solved, easily make glass-board surface be heated irregular, be difficult to control shaping glass sheets thickness problem.Especially by: 1800 ~ 1900 DEG C of sintering exceeding well-defined reaction temp, make siliconising react more abundant, ensure that the densification of material, avoid the cracking of product; In addition, sintered by high temperature oxidation, can check the STRESS VARIATION under the product condition of high temperature, the quality problems stopped in application process occur, and reduce application cost.
Certainly, implement arbitrary product of the present invention might not need to reach above-described all advantages simultaneously.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1, the manufacture method of the temperature-uniforming plate of the present embodiment comprises the following steps:
(1) prepare powder: after being mixed in the ratio of 1:2 with silicon carbide by carbon, the Zinic stearas adding 4% is lubricant, and the polyvinyl alcohol of 15% is caking agent, and mist projection granulating, obtains the powder of water content 5%.
(2) briquet is suppressed: after die-filling for powder tool, carry out shaped by fluid pressure with 200MPa pressing machine, obtain desired size briquet.
(3) biscuit is machining: the machine-shaping machining apparatus such as briquet brill, milling being completed biscuit.
(4) repair, dry: after molding biscuit being carried out to the finishing of surface imperfection, carry out the cryodrying of temperature 60 C, time 48h, then carry out temperature 80 DEG C, the time is the high temperature drying of 24h.
(5) vacuum sintering: smooth for the molding biscuit after high temperature drying being contained in scribbled on the graphite cake of boron nitride, and the silica flour placing relative base substrate weight 30% in the tiling of biscuit surface, dress vacuum electric furnace, carries out reaction sintering.Within the 36h time period, vacuumize intensification and be heated to 1800 DEG C, through siliconising, constant temperature, then fill helium and be cooled to 1200 DEG C, then inflated with nitrogen cools to less than 120 DEG C and comes out of the stove.
(6) impurity such as burning thing is accompanied to clear up, remove to the remnants on each surface of finished product of coming out of the stove.
(7) precise finiss processing: finished product of will the coming out of the stove employing machining center such as plane, milling carries out precise finiss processing, reaches physical dimension tolerance≤± 0.5mm, the requirement of upper and lower surfaceness≤6.3 μm.
(8) oxidation and sinter: the temperature-uniforming plate dress High Temperature Furnaces Heating Apparatus machined by precise finiss carries out oxidation and sinter.Within the 250h time period, be slowly warming up to 1100 DEG C, constant temperature 24h, then come out of the stove below slow cooling to 120 DEG C.
Embodiment 2, the manufacture method of the temperature-uniforming plate of the present embodiment comprises the following steps:
(1) prepare powder: after being mixed in the ratio of 1:5 with silicon carbide by carbon, the Zinic stearas adding 1% is lubricant, and the polyvinyl alcohol of 25% is caking agent, and mist projection granulating, obtains the powder of water content 2%.
(2) briquet is suppressed: after die-filling for powder tool, carry out shaped by fluid pressure with 200MPa pressing machine, obtain desired size briquet.
(3) biscuit is machining: the machine-shaping machining apparatus such as briquet brill, milling being completed biscuit.
(4) repair, dry: after molding biscuit being carried out to the finishing of surface imperfection, carry out the cryodrying of temperature 70 C, time 24h, then carry out temperature 100 DEG C, the time is the high temperature drying of 12h.
(5) vacuum sintering: smooth for the molding biscuit after high temperature drying being contained in scribbled on the graphite cake of boron nitride, and the silica flour placing relative base substrate weight 40% in the tiling of biscuit surface, dress vacuum electric furnace, carries out reaction sintering.Within the 28h time period, vacuumize intensification and be heated to 1900 DEG C, through siliconising, constant temperature, then fill helium and be cooled to 1100 DEG C, then inflated with nitrogen cools to less than 120 DEG C and comes out of the stove.
(6) impurity such as burning thing is accompanied to clear up, remove to the remnants on each surface of finished product of coming out of the stove.
(7) precise finiss processing: finished product of will the coming out of the stove employing machining center such as plane, milling carries out precise finiss processing, reaches physical dimension tolerance≤± 0.5mm, the requirement of upper and lower surfaceness≤6.3 μm.
(8) oxidation and sinter: the temperature-uniforming plate dress High Temperature Furnaces Heating Apparatus machined by precise finiss carries out oxidation and sinter.Within the 200h time period, be slowly warming up to 1200 DEG C, constant temperature 24h, then come out of the stove below slow cooling to 120 DEG C.
Embodiment 3, the manufacture method of the temperature-uniforming plate of the present embodiment comprises the following steps:
(1) prepare powder: after being mixed in the ratio of 1:4 with silicon carbide by carbon, the Zinic stearas adding 2% is lubricant, and the polyvinyl alcohol of 20% is caking agent, and mist projection granulating, obtains the powder of water content 3%.
(2) briquet is suppressed: after die-filling for powder tool, carry out shaped by fluid pressure with 200MPa pressing machine, obtain desired size briquet.
(3) biscuit is machining: the machine-shaping machining apparatus such as briquet brill, milling being completed biscuit.
(4) repair, dry: after molding biscuit being carried out to the finishing of surface imperfection, carry out the cryodrying of temperature 65 DEG C, time 36h, then carry out temperature 90 DEG C, the time is the high temperature drying of 18h.
(5) vacuum sintering: smooth for the molding biscuit after high temperature drying being contained in scribbled on the graphite cake of boron nitride, and the silica flour placing relative base substrate weight 35% in the tiling of biscuit surface, dress vacuum electric furnace, carries out reaction sintering.Within the 32h time period, vacuumize intensification and be heated to 1850 DEG C, through siliconising, constant temperature, then fill helium and be cooled to 1150 DEG C, then inflated with nitrogen cools to less than 120 DEG C and comes out of the stove.
(6) impurity such as burning thing is accompanied to clear up, remove to the remnants on each surface of finished product of coming out of the stove.
(7) precise finiss processing: finished product of will the coming out of the stove employing machining center such as plane, milling carries out precise finiss processing, reaches physical dimension tolerance≤± 0.5mm, the requirement of upper and lower surfaceness≤6.3 μm.
(8) oxidation and sinter: the temperature-uniforming plate dress High Temperature Furnaces Heating Apparatus machined by precise finiss carries out oxidation and sinter.Within the 230h time period, be slowly warming up to 1150 DEG C, constant temperature 24h, then come out of the stove below slow cooling to 120 DEG C.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (10)
1. reaction sintering silicon carbide ceramic temperature-uniforming plate, is characterized in that, its manufacture method comprises the following steps:
Prepare powder: by carbon with silicon carbide by 1:(2 ~ 5) mass ratio mix after, add the Zinic stearas of total mass 1% ~ 4% as lubricant, the polyvinyl alcohol of total mass 15% ~ 25% is as caking agent, and mist projection granulating, obtains powder;
Compacting briquet;
Vacuum sintering: the silica flour placing relative briquet weight 30 ~ 40% on briquet surface, carries out reaction sintering; Within 28 ~ 36h time period, vacuumize intensification and be heated to 1800 ~ 1900 DEG C, through siliconising, constant temperature, then fill helium and be cooled to 1100 ~ 1200 DEG C, then inflated with nitrogen cools to less than 120 DEG C;
Oxidation and sinter: the temperature-uniforming plate obtained is carried out oxidation and sinter; Within 200 ~ 250h time period, be slowly warming up to 1100 ~ 1200 DEG C, constant temperature 24h, then below slow cooling to 120 DEG C.
2. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, is characterized in that, describedly prepares in the step of powder, and the water content of the powder obtained is 2 ~ 5%.
3. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, it is characterized in that, the mass ratio of described carbon and silicon carbide is 1:4.
4. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, it is characterized in that, the add-on of described lubricant is 2% of total mass.
5. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, it is characterized in that, the add-on of described caking agent is 20% of total mass.
6. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, is characterized in that, also comprise the step of biscuit machine-shaping after the step of described compacting briquet.
7. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 6, is characterized in that, also comprise the step of finishing after the step of described biscuit machine-shaping, and the object of finishing is the surface imperfection eliminating biscuit.
8. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 7, it is characterized in that, the step of oven dry is also comprised after the step of described finishing, specifically comprise: the cryodrying carrying out temperature 60 ~ 70 DEG C, time 24 ~ 48h, carry out temperature 80 ~ 100 DEG C again, the time is the high temperature drying of 12 ~ 24h.
9. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 1, is characterized in that, also comprises the step of impurity cleaning after the step of described vacuum sintering, and impurity cleaning is to accompany burning thing impurity to remove to the remnants on each surface of finished product of coming out of the stove.
10. reaction sintering silicon carbide ceramic temperature-uniforming plate as claimed in claim 9, it is characterized in that, the step of attrition process is also comprised: reach physical dimension tolerance≤± 0.5mm after attrition process, upper and lower surfaceness≤6.3 μm after the step of described impurity cleaning.
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| CN201510334220.2A CN104926311A (en) | 2015-06-17 | 2015-06-17 | Reaction sintering silicon carbide ceramic uniform-temperature plate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673761A (en) * | 2017-10-27 | 2018-02-09 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of preparation method of big specification compact silicon carbide ceramic plate |
| CN110076882A (en) * | 2019-04-30 | 2019-08-02 | 董海明 | A kind of isostatic cool pressing composable mold and production method producing small micro- Ceramic Balls green body |
| CN111269016A (en) * | 2020-02-26 | 2020-06-12 | 上海德宝密封件有限公司 | Silicon carbide product sintering method |
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2015
- 2015-06-17 CN CN201510334220.2A patent/CN104926311A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673761A (en) * | 2017-10-27 | 2018-02-09 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of preparation method of big specification compact silicon carbide ceramic plate |
| CN107673761B (en) * | 2017-10-27 | 2021-05-04 | 潍坊华美精细技术陶瓷股份有限公司 | Preparation method of large-size compact silicon carbide ceramic plate |
| CN110076882A (en) * | 2019-04-30 | 2019-08-02 | 董海明 | A kind of isostatic cool pressing composable mold and production method producing small micro- Ceramic Balls green body |
| CN111269016A (en) * | 2020-02-26 | 2020-06-12 | 上海德宝密封件有限公司 | Silicon carbide product sintering method |
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Application publication date: 20150923 |