CN105036749A - Hot-pressing preparation method for hexagonal boron nitride-added silicon nitride - Google Patents
Hot-pressing preparation method for hexagonal boron nitride-added silicon nitride Download PDFInfo
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- CN105036749A CN105036749A CN201510374203.1A CN201510374203A CN105036749A CN 105036749 A CN105036749 A CN 105036749A CN 201510374203 A CN201510374203 A CN 201510374203A CN 105036749 A CN105036749 A CN 105036749A
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Abstract
The invention relates to a hot-pressing preparation method for hexagonal boron nitride-added silicon nitride. The preparation method comprises the following steps: adding hexagonal boron nitride having a laminar structure as a solid lubricating agent to silicon nitride, and mixing; meanwhile, adding a sintering aid and carrying out ball grinding; pouring alcohol to adjust the viscosity of fluid; then putting the ball-ground powder to a drying oven, heating, drying by steaming and sieving; then loading the powder to a die, and pre-pressing to form a biscuit; carrying out temperature preservation and pressure preservation in a vacuum carbon tube furnace; finally, reducing the temperature of the vacuum carbon tube furnace to room temperature, and taking sintered silicon nitride composite ceramic out. According to the preparation method disclosed by the invention, boron-containing oxides and hydroxides are generated by means of a chemical reaction between the hexagonal boron nitride and water molecules, so that the siding surface of a material has a lubricating property per se, and thus the tribological property of the silicon nitride ceramic material is remarkably improved, namely the friction factor of the silicon nitride ceramic material is remarkably reduced; the silicon nitride composite ceramic produced by hot-pressing sintering has the characteristics of good self-lubricating and tribological properties and can meet the using demands in actual engineering.
Description
Technical field
The present invention relates to ceramic materials preparation technology field, particularly a kind of silicon nitride adds the hot pressing method for preparing of hexagonal boron nitride.
Background technology
Silicon nitride (Si
3n
4) excellent physical mechanical property that stupalith has because of it, applied widely in engineering.In stupalith, the thermal expansivity of silicon nitride is little, so have good thermal shock resistance, its resistivity at room temperature is higher, can reach 10
13~ 10
14Ω cm, can as good insulating material; Silicon nitride chemical stability is fine, the corrosion of all mineral acids beyond hydrofluoric acid resistant and some alkali lye, also not infiltrate by molten metal alloys such as lead, aluminium, tin, silver, brass, nickel and corrosion, the silicon oxide film that during high temperature oxidation, its surface is formed can hinder further oxidation, oxidation resistance temperature reaches 1400 DEG C, and in reducing atmosphere, maximum operation (service) temperature can reach 1800 DEG C.
But pure silicon nitride stupalith can limit its engineer applied because of problems such as crisp rigid height, when simultaneously pure silicon nitride stupalith rubs under without medium lubricating condition, there are very high rubbing factor and wear rate, when especially joining pair with metal, its rubbing factor is up to 0.4-0.9, and wear rate is greater than 10
-6mm
3/ Nm.Conform to this situation, silicon nitride (Si
3n
4) sintex is when carrying out dry machining technology, crescent hollow abrasion, micro-tipping easily occur, and its tipping rate reaches 2% ~ 3%, causes quality and hidden trouble in safety.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, a kind of silicon nitride is the object of the present invention is to provide to add the hot pressing method for preparing of hexagonal boron nitride, be added in sintering procedure using the hexagonal boron nitride of lamellar structure as solid lubricant, the silicon nitride composite ceramics that hot pressed sintering is produced has self-lubricating, feature that tribological property is good.
In order to achieve the above object, the technical scheme that the present invention takes is:
Silicon nitride adds the hot pressing method for preparing of hexagonal boron nitride, and its step is as follows:
Step one: by volume ratio take the silicon nitride of 60% ~ 80%, the hexagonal boron nitride of 10% ~ 30% and 10% sintering aid powder, load weighted powder is placed in ball grinder and carries out ball mill mixing, pour alcohol into, add-on is that material is heavy by 1/2, regulate fluid viscosity, use planetary ball mill to make it fully mix, ball milling speed is 150rmin
-1, Ball-milling Time is 5 ~ 6h;
Step 2: the powder that ball milling is good is put and heats evaporate to dryness as in baking oven, evaporation limit, limit is stirred, until lose whole alcohol, prevents caking simultaneously, is ground by the compound after drying, and sieves with 160 eye mesh screens;
Step 3: thickness is that the graphite paper of 0.2mm is so that the demoulding on mould surrounding pad, powder is loaded in mould and is pressed into biscuit in advance, biscuit is placed in vacuum carbon tube furnace, under nitrogen protection, under temperature 1800 DEG C, pressure 30MPa condition, heat-insulation pressure keeping 30min;
Step 4: treat that vacuum carbon tube furnace furnace temperature is down to room temperature, open bell, takes out mould, take out in the sample from mould sintered, and take the graphite paper be bonded on sample off, the silicon nitride composite ceramics burnt till is taken out, detects its physical and mechanical property and tribological property.
Described silicon nitride granularity median size is 0.3 micron.
α-Si in described silicon nitride
3n
4purity be greater than 99.99%.
Described hexagonal boron nitride median size is 0.5 micron, and the purity of hexagonal boron nitride is greater than 99.6%.
Described sintering aid is Al
2o
3and Y
2o
3mixture, Al
2o
3and Y
2o
3median size is 1 micron, and purity is greater than 99.5%, Al
2o
3and Y
2o
3mass ratio be 1:1.
The present invention adopts hexagonal boron nitride as solid lubricant, generate containing boron oxide compound and oxyhydroxide by hexagonal boron nitride and water molecules generation chemical reaction, material sliding surface is made itself to have lubricity, thus improve the tribological property of silicon nitride ceramic material significantly, namely the rubbing factor of silicon nitride ceramic material is reduced, rubbing factor never adds during solid lubricant hexagonal boron nitride 0.5 ~ 0.6, be reduced to less than 0.1 after adding solid lubricant, the needs that Practical Project uses can be met.
Accompanying drawing explanation
Fig. 1 is the Si of hot pressed sintering
3n
4the XRD spectra of-20% hexagonal boron nitride ceramic composite.
Fig. 2 is the Si of hot pressed sintering
3n
4the corrosion surface shape appearance figure (SEM) of-20% hexagonal boron nitride ceramic composite.
Fig. 3 is Si
3n
4the fracture apperance figure (SEM) of-20% hexagonal boron nitride ceramic composite.
Fig. 4 is Si
3n
4the fracture apperance figure (SEM) of-10% hexagonal boron nitride ceramic composite.
Fig. 5 is Si
3n
4the fracture apperance figure (SEM) of-30% hexagonal boron nitride ceramic composite.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment one:
Step one: use electronic balance by volume ratio take the silicon nitride of 70%, the hexagonal boron nitride of 20% and 10% sintering aid powder, load weighted powder is placed in ball grinder and carries out ball mill mixing, pour alcohol into, add-on is that material is heavy by 1/2, regulate fluid viscosity, use planetary ball mill to make it fully mix, ball milling speed is 150rmin
-1, Ball-milling Time is about 5h;
Step 2: the powder that ball milling is good is put and heats evaporate to dryness as in baking oven, evaporation limit, limit is stirred, until lose whole alcohol, prevents caking simultaneously, is ground by the compound after drying, and sieves with 160 eye mesh screens;
Step 3: thickness is that the graphite paper of 0.2mm is so that the demoulding on mould surrounding pad, powder is loaded in mould and is pressed into biscuit in advance, biscuit is placed in vacuum carbon tube furnace, under nitrogen protection, under temperature 1800 DEG C, pressure 30MPa condition, heat-insulation pressure keeping 30min;
Step 4: treat that vacuum carbon tube furnace furnace temperature is down to room temperature, open bell, takes out mould, take out in the sample from mould sintered, and take the graphite paper be bonded on sample off, the silicon nitride composite ceramics burnt till is taken out, detects its physical and mechanical property and tribological property.
Described silicon nitride granularity median size is 0.3 micron, α-Si in silicon nitride
3n
4purity be greater than 99.99%.
Described hexagonal boron nitride median size is 0.5 micron, and the purity of hexagonal boron nitride is greater than 99.6%.
Described sintering aid is Al
2o
3and Y
2o
3mixture, Al
2o
3and Y
2o
3median size is 1 micron, and purity is greater than 99.5%, Al
2o
3and Y
2o
3mass ratio be 1:1.
See Fig. 1, by the Si of hot pressed sintering
3n
4the XRD spectra of-20% hexagonal boron nitride ceramic composite can be found out, Si
3n
4mainly β-the Si contained in-20% hexagonal boron nitride Ceramic Composite
3n
4with hBN phase, illustrate and can make α-Si at hot pressed sintering
3n
4be converted into β-Si
3n
4.
See Fig. 2, be the Si of hot pressed sintering
3n
4the corrosion surface shape appearance figure (SEM) of-20% hexagonal boron nitride ceramic composite, " A ", " B " 2 in Fig. 2 is carried out to the energy spectrum analysis (EDS analysis) of specimen surface composition, analytical results is in table 1:
Table 1Si
3n
4the energy spectrum analysis (EDS) of-20%hBN specimen surface composition
β-the Si that in Fig. 2, " A " is column
3n
4, the hBN that " B " is lamellar, as can be seen from Table 1: the Si content in " A " region is apparently higher than " B " region, and the B content in " B " region is significantly higher than " A " region, and this confirms further " A " is Si
3n
4region, " B " is hBN region.
The mechanical property of the silicon nitride composite ceramics that the present embodiment one obtains is as following table 2:
Table 2 hot pressed sintering Si
3n
4the physical and mechanical property of-hBN sample
See Fig. 3 and table 2, can draw to draw a conclusion: add the hBN of 20%, Si
3n
4the density of pottery declines, and ceramic density never adds 3.30gcm during hBN
3drop to 2.97gcm
3, rubbing factor drops to 0.19 from 0.50 ~ 0.60, and frictional behaviour improves obviously.
Embodiment two:
Step one: use electronic balance by volume ratio take the silicon nitride of 60%, the hexagonal boron nitride of 30% and 10% sintering aid powder, load weighted powder is placed in ball grinder and carries out ball mill mixing, pour alcohol into, add-on is that material is heavy by 1/2, regulate fluid viscosity, use planetary ball mill to make it fully mix, ball milling speed is 150rmin
-1, Ball-milling Time is about 5.5h;
Step 2: the powder that ball milling is good is put and heats evaporate to dryness as in baking oven, evaporation limit, limit is stirred, until lose whole alcohol, prevents caking simultaneously, is ground by the compound after drying, and sieves with 160 eye mesh screens;
Step 3: thickness is that the graphite paper of 0.2mm is so that the demoulding on mould surrounding pad, powder is loaded in mould and is pressed into biscuit in advance, biscuit is placed in vacuum carbon tube furnace, under nitrogen protection, under temperature 1800 DEG C, pressure 30MPa condition, heat-insulation pressure keeping 30min;
Step 4: treat that vacuum carbon tube furnace furnace temperature is down to room temperature, open bell, takes out mould, take out in the sample from mould sintered, and take the graphite paper be bonded on sample off, the silicon nitride composite ceramics burnt till is taken out, detects its physical and mechanical property and tribological property.
Described silicon nitride granularity median size is 0.3 micron, α-Si in silicon nitride
3n
4purity be greater than 99.99%.
Described hexagonal boron nitride median size is 0.5 micron, and the purity of hexagonal boron nitride is greater than 99.6%.
Described sintering aid is Al
2o
3and Y
2o
3mixture, Al
2o
3and Y
2o
3median size is 1 micron, and purity is greater than 99.5%, Al
2o
3and Y
2o
3mass ratio be 1:1.
The mechanical property of the silicon nitride composite ceramics that the present embodiment two obtains is as following table 3:
Table 3 hot pressed sintering Si
3n
4the physical and mechanical property of-hBN sample
See Fig. 4 and table 3, can draw to draw a conclusion: add the hBN of 30%, Si
3n
4the density of pottery declines, and ceramic density never adds 3.30gcm during hBN
3drop to 2.94gcm
3, rubbing factor drops to 0.15 from 0.50 ~ 0.60, and frictional behaviour improves obviously.
Embodiment three:
Step one: use electronic balance by volume ratio take the silicon nitride of 80%, the hexagonal boron nitride of 10% and 10% sintering aid powder, load weighted powder is placed in ball grinder and carries out ball mill mixing, pour alcohol into, add-on is that material is heavy by 1/2, regulate fluid viscosity, use planetary ball mill to make it fully mix, ball milling speed is 150rmin
-1, Ball-milling Time is about 6h;
Step 2: the powder that ball milling is good is put and heats evaporate to dryness as in baking oven, evaporation limit, limit is stirred, until lose whole alcohol, prevents caking simultaneously, is ground by the compound after drying, and sieves with 160 eye mesh screens;
Step 3: thickness is that the graphite paper of 0.2mm is so that the demoulding on mould surrounding pad, powder is loaded in mould and is pressed into biscuit in advance, biscuit is placed in vacuum carbon tube furnace, under nitrogen protection, under temperature 1800 DEG C, pressure 30MPa condition, heat-insulation pressure keeping 30min;
Step 4: treat that vacuum carbon tube furnace furnace temperature is down to room temperature, open bell, takes out mould, take out in the sample from mould sintered, and take the graphite paper be bonded on sample off, the silicon nitride composite ceramics burnt till is taken out, detects its physical and mechanical property and tribological property.
Described silicon nitride granularity median size is 0.3 micron, α-Si in silicon nitride
3n
4purity be greater than 99.99%.
Described hexagonal boron nitride median size is 0.5 micron, and the purity of hexagonal boron nitride is greater than 99.6%.
Described sintering aid is Al
2o
3and Y
2o
3mixture, Al
2o
3and Y
2o
3median size is 1 micron, and purity is greater than 99.5%, Al
2o
3and Y
2o
3mass ratio be 1:1.
The mechanical property of the silicon nitride composite ceramics that the present embodiment three obtains is as following table 4:
Table 4 hot pressed sintering Si
3n
4the physical and mechanical property of-hBN sample
See Fig. 5 and table 4, can draw to draw a conclusion: add the hBN of 10%, Si
3n
4the density of pottery declines, and ceramic density never adds 3.30gcm during hBN
3drop to 3.10gcm
3, rubbing factor drops to 0.20 from 0.50 ~ 0.60, and frictional behaviour improves obviously.
Claims (5)
1. silicon nitride adds the hot pressing method for preparing of hexagonal boron nitride, and it is characterized in that, step is as follows:
Step one: by volume ratio take the silicon nitride of 60% ~ 80%, the hexagonal boron nitride of 10% ~ 30% and 10% sintering aid powder, load weighted powder is placed in ball grinder and carries out ball mill mixing, pour alcohol into, add-on is that material is heavy by 1/2, regulate fluid viscosity, use planetary ball mill to make it fully mix, ball milling speed is 150rmin
- 1, Ball-milling Time is 5 ~ 6h;
Step 2: the powder that ball milling is good is put and heats evaporate to dryness as in baking oven, evaporation limit, limit is stirred, until lose whole alcohol, prevents caking simultaneously, is ground by the compound after drying, and sieves with 160 eye mesh screens;
Step 3: thickness is that the graphite paper of 0.2mm is so that the demoulding on mould surrounding pad, powder is loaded in mould and is pressed into biscuit in advance, biscuit is placed in vacuum carbon tube furnace, under nitrogen protection, under temperature 1800 DEG C, pressure 30MPa condition, heat-insulation pressure keeping 30min;
Step 4: treat that vacuum carbon tube furnace furnace temperature is down to room temperature, open bell, takes out mould, take out in the sample from mould sintered, and take the graphite paper be bonded on sample off, the silicon nitride composite ceramics burnt till is taken out, detects its physical and mechanical property and tribological property.
2. silicon nitride according to claim 1 adds the hot pressing method for preparing of hexagonal boron nitride, and it is characterized in that, described silicon nitride granularity median size is 0.3 micron.
3. silicon nitride according to claim 1 adds the hot pressing method for preparing of hexagonal boron nitride, it is characterized in that, α-Si in described silicon nitride
3n
4purity be greater than 99.99%.
4. silicon nitride according to claim 1 adds the hot pressing method for preparing of hexagonal boron nitride, and it is characterized in that, described hexagonal boron nitride median size is 0.5 micron, and the purity of hexagonal boron nitride is greater than 99.6%.
5. the silicon nitride according to the arbitrary claim of claim 1-4 adds the hot pressing method for preparing of hexagonal boron nitride, and it is characterized in that, described sintering aid is Al
2o
3and Y
2o
3mixture, Al
2o
3and Y
2o
3median size is 1 micron, and purity is greater than 99.5%, Al
2o
3and Y
2o
3mass ratio be 1:1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117396A (en) * | 2017-12-11 | 2018-06-05 | 陕西科技大学 | The preparation method of biomedical ceramics material based on silicon nitride |
| CN109357531A (en) * | 2018-10-09 | 2019-02-19 | 牡丹江师范学院 | A kind of agglomerating plant and its sintering method for cubic boron nitride sintered body |
| CN109400173A (en) * | 2018-10-30 | 2019-03-01 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride fiber enhancing nitride ceramic composites and preparation method thereof |
| CN110698207A (en) * | 2019-11-08 | 2020-01-17 | 陕西科技大学 | Silicon nitride-based layered ceramic composite material and preparation method thereof |
| CN112430100A (en) * | 2020-12-10 | 2021-03-02 | 山东鹏程陶瓷新材料科技有限公司 | Si3N4-BN complex phase ceramic and preparation method thereof |
| CN113614035A (en) * | 2019-03-29 | 2021-11-05 | 电化株式会社 | Silicon nitride powder, method for producing same, and method for producing silicon nitride sintered body |
| CN114292111A (en) * | 2021-12-28 | 2022-04-08 | 海南大学 | Compact silicon nitride/hexagonal boron nitride composite ceramic and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117396A (en) * | 2017-12-11 | 2018-06-05 | 陕西科技大学 | The preparation method of biomedical ceramics material based on silicon nitride |
| CN109357531A (en) * | 2018-10-09 | 2019-02-19 | 牡丹江师范学院 | A kind of agglomerating plant and its sintering method for cubic boron nitride sintered body |
| CN109400173A (en) * | 2018-10-30 | 2019-03-01 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride fiber enhancing nitride ceramic composites and preparation method thereof |
| CN109400173B (en) * | 2018-10-30 | 2021-09-10 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber reinforced nitride composite material and preparation method thereof |
| CN113614035A (en) * | 2019-03-29 | 2021-11-05 | 电化株式会社 | Silicon nitride powder, method for producing same, and method for producing silicon nitride sintered body |
| CN110698207A (en) * | 2019-11-08 | 2020-01-17 | 陕西科技大学 | Silicon nitride-based layered ceramic composite material and preparation method thereof |
| CN112430100A (en) * | 2020-12-10 | 2021-03-02 | 山东鹏程陶瓷新材料科技有限公司 | Si3N4-BN complex phase ceramic and preparation method thereof |
| CN114292111A (en) * | 2021-12-28 | 2022-04-08 | 海南大学 | Compact silicon nitride/hexagonal boron nitride composite ceramic and preparation method thereof |
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Application publication date: 20151111 |