CN100567215C - The preparation method of a kind of high heat conduction, high breaking strength niberlox - Google Patents
The preparation method of a kind of high heat conduction, high breaking strength niberlox Download PDFInfo
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- CN100567215C CN100567215C CNB2008100451481A CN200810045148A CN100567215C CN 100567215 C CN100567215 C CN 100567215C CN B2008100451481 A CNB2008100451481 A CN B2008100451481A CN 200810045148 A CN200810045148 A CN 200810045148A CN 100567215 C CN100567215 C CN 100567215C
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Abstract
The invention belongs to electric function ceramic material technology field, relate to the preparation method of niberlox.The present invention adopts BeO raw material and sintering agent to disperse respectively and the mode of grinding is controlled raw material particle size, adopt the wet-milling mode with the two uniform mixing then, adopt the syllogic sintering processing sintering of uniqueness of the present invention after drying, granulation and the moulding: at first between 1000 ℃ to 1400 ℃, be incubated 0.5～4 hour, heat-up rate with 3 ℃～8 ℃/min is warmed up between 1620 ℃ to 1680 ℃ then, and last fast cooling to 1520 ℃ is between 1580 ℃ and be incubated 2～6 hours.BeO ceramic crystalline grain controlled amount, consistence and good reproducibility that the present invention is prepared; Adopt unique syllogic sintering processing, make final BeO ceramic structure even compact, thereby improved the thermal conductivity and the folding strength of final BeO stupalith.The BeO stupalith of the present invention preparation is as high heat conduction main body critical material, can be used for playing carrying heat conduction function in the electronic devices and components of microwave, millimeter wave, high-power, high assembled density or the assembly.
Description
Technical field
The invention belongs to electric function ceramic material technology field, particularly the preparation method of niberlox.
Background technology
Along with the raising day by day of electronic functionalities, electron device develops to miniaturization, multifunction, high-power direction, and heat dissipation, the stress relief of electron device proposed more and more higher requirement.Analysis revealed according to statistics, in causing the electronic product failure reasons: heat dissipation problem accounts for 55%, and vibration problem accounts for 20%, and the envrionment temperature problem accounts for 19%, and dust problems accounts for 6%.Though can make heat distribution as far as possible rationally by optimization design, the stress that vibration is produced discharges as far as possible, tackle the problem at its root needs to adopt the material of high thermal conductance, high breaking strength.
The BeO stupalith is high heat conduction main body critical material, is used widely in the electronic devices and components of microwave, millimeter wave, high-power, high assembled density or assembly, plays carrying heat conduction function.At present, the making method of domestic BeO stupalith main manufacturer employing as shown in Figure 1.In this preparation method be that half-dried powder mixes because porcelain preparation adopts, raw material be not even especially mixing of sintering agent, stupalith crystal grain is grown up unusually easily and is not of uniform size, product performance are dispersed big, consistence, repeated bad; Add that mixed powder will carry out pre-burning, calcined temperature is about 1400 ℃, and the porcelain activity is lower; BeO ceramic sintering temperature height, more than 1750 ℃, energy consumption is bigger usually.
In order to overcome above-mentioned shortcoming, the making of the U.S. BeO of Brush company stupalith is adopted as Fig. 2 making method.
Compare with method shown in Figure 1, this method makes ceramic sintering temperature lower, and homogeneity of product, repeatability are greatly improved.But because the addition of sintering agent is very little, usually below 0.5%, a spot of sintering agent still is not easy homodisperse, and product grains is still grown up easily unusually, and phenomenon not of uniform size is ubiquity still.Add and adopt conventional sintering technology, promptly be raised to top temperature with certain temperature rise rate after the insulation regular hour make ceramic densifying.Under top temperature, crystal boundary obtains bigger thrust, and pottery crystal boundary in densification process is crossed pore easily makes pore wrap into the inside of crystal grain, causes the product density to be difficult to improve, thereby influences the raising of BeO ceramic performance.
Summary of the invention
The invention provides that a kind of preparation technology is simple, energy consumption is lower, sintering method is easily controlled, and BeO ceramic crystalline grain controlled amount, even structure densification, have the niberlox preparation method of high heat conductance and high breaking strength.
The high heat conductance that the present invention proposes, the preparation method of high breaking strength BeO stupalith comprise the steps: as shown in Figure 3
The preparation of step 1, porcelain green compact specifically comprises step by step following:
Step 1 is disperseed sintering agents such as BeO raw material and Mg, Al, Si respectively and is ground to form slurry.The mean particle size of control BeO raw material slurry is below 1.0 μ m, and concentration is between 30～60%; The mean particle size of control sintering agent slurry is below 0.5 μ m, and concentration is between 1～30%.
In the dispersion and process of lapping of above-mentioned BeO raw material and sintering agents such as Mg, Al, Si, disperse and lapping mode can be taked ball milling, the mode that stirs mill, vibration or sand milling is disperseed and grind; Dispersion liquid can adopt one or more in deionized water, ethanol, the Virahol; Can also add one or more properties-correcting agent such as methylcellulose gum, Acidum Citricum or polyacrylamide in the dispersion process.
Step 2 is injected into the sintering agent slurry of step 1 gained in the slurry of BeO raw material of step 1 gained mix grinding more by a certain percentage, and specifically injection ratio is 0.5% of the sintering agent slurry sintering agent content contained BeO raw materials quality of slurry that is no more than the BeO raw material.
Above-mentioned mix grinding mode can be a ball milling, and the time is 5～20 hours; Also can be vibration, stir mill or sand milling, the time be 0.5～4 hour.
Step 3 is mixed slurry oven dry, the granulation of the BeO raw material of step 2 gained and sintering agent, according to the required shape moulding of reality.
Concrete bake out temperature can be between 80 ℃-150 ℃.
Step 2, the porcelain green compact of step 1 gained are taked syllogic sintering processing sintering, specifically comprise step by step following:
Step 4 fs sintering: heat preservation sintering is 0.5～4 hour under the temperature condition between 1000 ℃ to 1400 ℃, make and produce bonding between the powdery particles of porcelain green compact, the contact area of particulate evenly increases, and the center of particulate is close mutually, live in concentrated communities, and produces crystal boundary between the small grains.
Step 5 subordinate phase sintering: after the fs, sintering was finished, be warmed up between 1620 ℃ to 1680 ℃, make crystal boundary obtain bigger thrust with the heat-up rate of 3 ℃～8 ℃/min.
Step 6 phase III sintering: after the subordinate phase sintering is finished, fast cooling to 1520 ℃ is between 1580 ℃ and heat preservation sintering 2～6 hours, crystal boundary obtains bigger thrust in the subordinate phase sintering process after, be with pore to advance together, do not make pore wrap into the inside of crystal grain, make in the sintered compact the original hole that is communicated with not section dwindle, final pore is excluded, and realizes the densification of sintered compact.
Above-mentioned temperature fall time from the subordinate phase sintering temperature to the phase III sintering temperature preferably is no more than 30 minutes; The heat preservation sintering process of phase III can be carried out in air or in the reducing atmosphere.
The invention has the beneficial effects as follows: the mode of 1, taking BeO raw material and Mg, Al, Si sintering agent to disperse respectively and grind, the particle diameter of BeO raw material and Mg, Al, Si sintering agent is controlled respectively, accomplish the particle diameter homogeneous and controllable of raw material, thereby guarantee final BeO ceramic crystalline grain controlled amount; 2, take BeO raw material and Mg, Al, Si sintering agent wet method mix grinding to get mode, it is very even to make that BeO raw material and Mg, Al, Si sintering agent mix, thereby guarantees the consistence and the good reproducibility of the finished product; 3, adopt unique syllogic sintering processing, help the eliminating of pore, make final BeO ceramic structure even compact, thereby improved the thermal conductivity and the folding strength of final BeO stupalith.
Description of drawings
Preparation method's schema of the present domestic BeO stupalith of Fig. 1.
Preparation method's schema of the BeO stupalith that Fig. 2 U.S. Brush company produces.
Preparation method's schema of Fig. 3 high heat conductance of the present invention, high breaking strength niberlox.
The SEM figure of the beryllium oxide ceramics sample of Fig. 4 specific embodiment of the invention 1 gained.
The SEM figure of the beryllium oxide ceramics sample of Fig. 5 specific embodiment of the invention 2 gained.
The SEM figure of the beryllium oxide ceramics sample of Fig. 6 specific embodiment of the invention 3 gained.
Embodiment
Embodiment 1
Get MgO powder 100 gram and SiO
2Powder 150 gram places ball grinder to be the dispersion liquid ball milling with ethanol (1250 gram) and obtains the A slurry to the mean particle size of slurry below 0.5 μ m; Getting 20 kilograms of 99BeO raw materials is that dispersion liquid stirs the mean particle size be milled to slurry obtain the B slurry below 1.0 μ m with deionized water (20～25 kilograms).Then 600 gram A slurries are injected the stirring mill that whole B slurry carried out 1.5 hours again, with mean particle size in the oven dry of the following mixed slurry of 0.8 μ m, granulation, moulding obtains raw cook, be not incubated after 1000 ℃ down insulation was raised to 1680 ℃ in 3.5 hours fast drop to rapidly 1580 ℃ down 2 hours sintering of insulation obtain 99 beryllium oxide ceramics sample C1.The C1 various aspects of performance is as shown in table 1, and its SEM figure as shown in Figure 4.
Embodiment 2
Get MgO powder 100 gram and SiO
2Powder 150 gram places ball grinder to be the dispersion liquid ball milling with Virahol (1250 gram) and obtains the A slurry to the mean particle size of slurry below 0.5 μ m; Getting 20 kilograms of 99BeO raw materials is that dispersion liquid stirs the mean particle size be milled to slurry obtain the B slurry below 1.0 μ m with deionized water (20～25 kilograms).Then 600 gram A slurries are injected the ball milling that whole B slurry carried out 8 hours again, with mean particle size in the oven dry of the following mixed slurry of 0.8 μ m, granulation, moulding obtains raw cook, be not incubated after 1400 ℃ down insulation was raised to 1620 ℃ in 1 hour fast drop to rapidly 1520 ℃ down 6 hours sintering of insulation obtain 99 beryllium oxide ceramics sample C2.The C2 various aspects of performance is as shown in table 1, and its SEM figure as shown in Figure 5.
Embodiment 3
Get MgO powder 100 gram and SiO
2Powder 150 gram places ball grinder to be the dispersion liquid ball milling with deionized water (1250 gram) and obtains the A slurry to the mean particle size of slurry below 0.5 μ m; Getting 20 kilograms of 99BeO raw materials is that dispersion liquid stirs the mean particle size be milled to slurry obtain the B slurry below 1.0 μ m with deionized water (20～25 kilograms).Then 600 gram A slurries are injected the ball milling that whole B slurry carried out 15 hours again, with mean particle size in the oven dry of the following mixed slurry of 0.8 μ m, granulation, moulding obtains raw cook, be not incubated after 1200 ℃ down insulation was raised to 1650 ℃ in 2 hours fast drop to rapidly 1550 ℃ down 4 hours sintering of insulation obtain 99 beryllium oxide ceramics sample C3.The C3 various aspects of performance is as shown in table 1, and its SEM figure as shown in Figure 6.
The performance of table 1 beryllium oxide ceramics sample
| Sample | Density (g/cm3) | Thermal conductivity (W/mk) | Bending strength (Mpa) |
| C1 | 2.951 | 298 | 235 |
| C2 | 2.938 | 293 | 238 |
| C3 | 2.942 | 295 | 236 |
Claims (6)
1, the preparation method of a kind of high heat conductance, high breaking strength niberlox is characterized in that, comprises the steps:
The preparation of step 1, porcelain green compact specifically comprises step by step following:
Step 1 is disperseed BeO raw material and Mg, Al, Si sintering agent respectively and is ground to form slurry; The mean particle size of control BeO raw material slurry is below 1.0 μ m, and concentration is between 30～60%; The mean particle size of control sintering agent slurry is below 0.5 μ m, and concentration is between 1～30%;
Step 2 is injected into the sintering agent slurry of step 1 gained in the slurry of BeO raw material of step 1 gained mix grinding more by a certain percentage, and specifically injection ratio is 0.5% of the sintering agent slurry sintering agent content contained BeO raw materials quality of slurry that is no more than the BeO raw material;
Step 3 is mixed slurry oven dry, the granulation of the BeO raw material of step 2 gained and sintering agent, according to the required shape moulding of reality;
Step 2, the porcelain green compact of step 1 gained are taked syllogic sintering processing sintering, specifically comprise step by step following:
Step 4 fs sintering: heat preservation sintering is 0.5～4 hour under the temperature condition between 1000 ℃ to 1400 ℃, make and produce bonding between the powdery particles of porcelain green compact, the contact area of particulate evenly increases, and the center of particulate is close mutually, live in concentrated communities, and produces crystal boundary between the small grains;
Step 5 subordinate phase sintering: after the fs, sintering was finished, be warmed up between 1620 ℃ to 1680 ℃, make crystal boundary obtain bigger thrust with the heat-up rate of 3 ℃～8 ℃/min;
Step 6 phase III sintering: after the subordinate phase sintering is finished, fast cooling to 1520 ℃ is between 1580 ℃ and heat preservation sintering 2～6 hours, crystal boundary obtains bigger thrust in the subordinate phase sintering process after, be with pore to advance together, do not make pore wrap into the inside of crystal grain, the hole of original connection in the sintered compact is constantly dwindled, and final pore is excluded, and realizes the densification of sintered compact.
2, the preparation method of high heat conductance according to claim 1, high breaking strength niberlox, it is characterized in that, step by step in 1 in the dispersion and process of lapping of BeO raw material and Mg, Al, Si sintering agent of described step 1 disperses and lapping mode is taked ball milling, the mode that stirs mill, vibration or sand milling is disperseed and grind; Dispersion liquid adopts more than one in deionized water, ethanol, the Virahol; Add more than one properties-correcting agent of methylcellulose gum, citric acid or polyacrylamide in the dispersion process.
3, the preparation method of high heat conductance according to claim 1 and 2, high breaking strength niberlox is characterized in that, the mix grinding mode in 2 step by step of described step 1 is a ball milling, and the time is 5～20 hours.
4, the preparation method of high heat conductance according to claim 1 and 2, high breaking strength niberlox is characterized in that, the mix grinding mode in 2 step by step of described step 1 is vibration, stirs mill or sand milling, and the time is 0.5～4 hour.
5, the preparation method of high heat conductance according to claim 1 and 2, high breaking strength niberlox is characterized in that, the concrete bake out temperature in 3 step by step of described step 1 is between 80 ℃-150 ℃.
6, the preparation method of high heat conductance according to claim 1 and 2, high breaking strength niberlox, it is characterized in that the temperature fall time from the subordinate phase sintering temperature to the phase III sintering temperature in 5 step by step of described step 2 is no more than 30 minutes; The heat preservation sintering process of phase III is carried out in air or in the reducing atmosphere.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101462867B (en) * | 2009-01-16 | 2011-09-14 | 中南大学 | Method for preparing BeO ceramic by gel injection moulding forming technique |
| CN104556979B (en) * | 2014-12-26 | 2016-06-08 | 宜宾红星电子有限公司 | A kind of beryllium oxide ceramics supporting rod and preparation method thereof |
| CN108623288B (en) * | 2018-06-21 | 2021-08-06 | 宜宾红星电子有限公司 | Beryllium oxide ceramic tape-casting slurry and production method thereof |
| CN109053160A (en) * | 2018-08-27 | 2018-12-21 | 芜湖市元奎新材料科技有限公司 | A kind of preparation method of high breaking strength beryllium oxide ceramics |
| CN110105055B (en) * | 2019-06-20 | 2021-08-24 | 宜宾红星电子有限公司 | Method for manufacturing beryllium oxide ceramic polished substrate for thin film circuit |
| CN113800892A (en) * | 2021-09-24 | 2021-12-17 | 宜宾红星电子有限公司 | Forming method for fine structure beryllium oxide ceramic |
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Non-Patent Citations (4)
| Title |
|---|
| 烧结助剂和工艺对BeO 陶瓷密度和热导率的影响. 文丹华等.粉末冶金材料科学与工程，第12卷第5期. 2007 |
| 烧结助剂和工艺对BeO 陶瓷密度和热导率的影响. 文丹华等.粉末冶金材料科学与工程，第12卷第5期. 2007 * |
| 高纯高导热BeO 陶瓷材料烧结工艺研究. 钟朝位等.压电与声光，第29卷第6期. 2007 |
| 高纯高导热BeO 陶瓷材料烧结工艺研究. 钟朝位等.压电与声光，第29卷第6期. 2007 * |
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