CN108395255A - A kind of aluminium nitride composite material and preparation method thereof and the application in vehicle exhaust temperature sensor - Google Patents
A kind of aluminium nitride composite material and preparation method thereof and the application in vehicle exhaust temperature sensor Download PDFInfo
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Abstract
The invention belongs to field of inorganic nonmetallic material, specifically a kind of aluminium nitride composite material and preparation method thereof and the applications in automobile exhaust sensor.The aluminium nitride composite material is made of the material composition of following mass percent：60~80wt% of aluminium nitride, 20~35wt% of silica, 0~10 wt% of sintering aid, the sum of each Ingredient Amount are 100%.The present invention selects aluminium nitride composite material to substitute magnesia as embedding packing material, and the thermal response time of vehicle exhaust temperature sensor is improved with this, can be promoted within 5 seconds.Aluminium nitride composite material obtained by the present invention is as embedding packing material, it contains suitable sintering aid and silica in component is promoted to melt and fill aluminium nitride molecular gap, the thermal conductivity for improving packing material ensure that the vehicle exhaust temperature sensor response time is the requirement within 5s.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, and in particular to a kind of aluminium nitride composite material and preparation method thereof with
And the application in automobile exhaust sensor.
Background technology
The response time of existing vehicle exhaust temperature sensor is 10s or so.If necessary to more timely feedback signal,
The response time of existing sensor further must be promoted, and is preferably controlled within 5s.
Existing vehicle exhaust temperature sensor generally uses magnesia as embedding packing material.And the thermal conductivity of magnesia
Rate only about 36W/m K require the higher response time now for vehicle exhaust temperature sensor, this is just to embedding packing material
Thermal conductivity more stringent requirements are proposed.Therefore, it is to be difficult to meet present vehicle exhaust using magnesia as embedding packing material
The temperature sensor response time is the requirement within 5s.
For this purpose, being badly in need of developing a kind of embedding packing material with high heat conductance.
Aluminium nitride（AlN）Material is a kind of good heat shock resistance material, with high thermal conductivity（About 320W/m K）
With low coefficient of thermal expansion（4.5×10-6℃）.Chinese patent CN 1666307A disclose a kind of stabilization with tungsten/aluminium nitride
Pyrostat/heater system and method, it includes have AlN substrate.Chinese patent CN 102853926A disclose one kind
Nitridation may be selected in the encapsulating structure and its manufacturing method of MEMS temperature sensor, MEMS substrate material and film sealing cap material
Aluminium.As it can be seen that aluminium nitride material is applied in temperature sensor field.
Certainly, in the application field of vehicle exhaust temperature sensor, also there are the patent report that aluminium nitride material is applied, example
If Chinese patent CN 204346594U disclose a kind of vehicle exhaust pyrostat, high temperature conducting region is equipped in structure
And insulation layer, aluminium nitride or boron nitride powder are filled with around the temperature detecting element in high temperature conducting region, and insulating
Area is filled with magnesia or alumina powder.However the patent be only be simply filled with, and for the sealing performance of embedding how
Do not considered.And Chinese patent CN 101144002A disclose a kind of temperature sensor imbedding material, consider for
The leakproofness of embedding, but it refers to modified epoxy, belongs to high molecular material, can reach -30 DEG C（5 minutes oil
In）-120℃（In 5 minutes oil）1000 temperature shocks, and the Embedding Material of the present invention is field of inorganic materials, the two
Use temperature range is entirely different.
Invention content
The present invention is difficult to meet vehicle exhaust temperature for existing magnesia embedding packing material present in background technology
This technical problem of the higher requirement of sensor and a kind of aluminium nitride composite material is provided.The aluminium nitride composite material has
High thermal conductivity disclosure satisfy that the requirement in the corresponding time 5s of vehicle exhaust pyrostat.
Another object of the present invention is to provide a kind of preparation methods of aluminium nitride composite material.
It is still another object of the present invention to provide a kind of aluminium nitride composite material answering in vehicle exhaust temperature sensor
With.
Realize an of the invention purpose and the technical solution that uses for：A kind of aluminium nitride composite material, by following quality hundred
The material composition of ratio is divided to be made：60~80wt% of aluminium nitride, 20~35wt% of silica, 0~10 wt% of sintering aid, each ingredient
The sum of dosage is 100%.
As a preferred embodiment of the invention, sintering aid of the present invention is aluminium oxide.
As a preferred embodiment of the invention, sintering aid of the present invention is modified oxidized aluminium composite material.
As a preferred embodiment of the invention, modified oxidized aluminium composite material of the present invention, by following parts by weight
Raw material be made：40~60 parts of aluminium oxide, 3~8 parts of nano zine oxide, 10~20 parts of silicon powder, 5~10 parts of magnesia.
As a preferred embodiment of the invention, modified oxidized aluminium composite material of the present invention is by following preparation process
It is made：
1）In proportion by aluminium oxide, nano zine oxide, silicon powder, magnesia carry out ball milling mixing, mill speed be 200~
250r/min, Ball-milling Time are 2~3h, and the ball-milling medium that ball milling is selected is that the mixing of absolute ethyl alcohol-water-hydroxymethyl cellulose is molten
Liquid, the aluminium oxide, nano zine oxide, silicon powder, the quality sum of magnesia and ball-milling medium mass volume ratio 1g：1~
5mL, the absolute ethyl alcohol-water-hydroxymethyl cellulose mixed solution press absolute ethyl alcohol：Water：Hydroxymethyl cellulose presses quality volume
Compare 1mL：1mL：2g is formulated, and mixed slurry is made；
2）By step 1）Mixed slurry obtained is first dried, and then re-sinters, and obtains modified oxidized aluminium composite material；It burns
Junction temperature is 520~530 DEG C, and sintering time is 1~3 hour.
Realize an of the invention purpose and a kind of technical solution for using for：A kind of preparation method of aluminium nitride composite material,
Its preparation process is：
1）AlN-SiO2The preparation of matrix slurry；
Aluminium nitride, silica and sintering aid are uniformly mixed in proportion, absolute ethyl alcohol is added and carries out ball milling, AlN- is made
SiO2Matrix slurry；
2）AlN-SiO2The preparation of matrix composite powder；
By step 1）AlN-SiO obtained2The drying of matrix slurry grinds and is sieved, and AlN-SiO is made2Matrix composite powder.
Wherein, in step 1）In, the sum of the aluminium nitride, silica and sintering aid weight press matter with absolute ethyl alcohol
Amount is than being 1：1, Ball-milling Time is 0.5~2 hour；Step 2）Described in drying temperature be 80~100 DEG C, drying time 6
~10 hours, sieving screening size was 300~350 mesh.
Realize an of the invention purpose and the another technical solution that uses for：A kind of preparation side of aluminium nitride composite material
Method, preparation process are：
1）The preparation of modified oxidized aluminium composite material
Aluminium oxide, nano zine oxide, silicon powder, magnesia are subjected to ball milling mixing in proportion, mill speed is 200~250r/
Min, Ball-milling Time are 2~3h, and the ball-milling medium that ball milling is selected is the mixed solution of absolute ethyl alcohol-water-hydroxymethyl cellulose, institute
State the mass volume ratio 1g of aluminium oxide, nano zine oxide, silicon powder, the quality sum of magnesia and ball-milling medium：1~10mL,
Mixed slurry is made；
Mixed slurry obtained is first dried, is then re-sintered, modified oxidized aluminium composite material is obtained；Sintering temperature is
520~530 DEG C, sintering time is 1~3 hour；
2）AlN-SiO2The preparation of matrix slurry；
In proportion by aluminium nitride, silica and step 1）Modified oxidized aluminium composite material obtained is uniformly mixed, and is added anhydrous
Ethyl alcohol carries out ball milling, and AlN- SiO are made2Matrix slurry；
3）AlN-SiO2The preparation of matrix composite powder；
Step 2 is added in epoxy resin and ethylenediamine in proportion）AlN-SiO obtained2In matrix slurry, normal temperature cure is carried out,
Hardening time is 0.5~2 hour, is ground up, sieved after drying, and AlN-SiO is made2Matrix composite powder.
Realize still a further object of the present invention and the technical solution that uses for：A kind of aluminium nitride composite material is in vehicle exhaust temperature
Aluminium nitride composite material is packed into vehicle exhaust temperature sensor and is used as Embedding Material by the application in sensor, and
It is sintered under 600~800 DEG C of temperature condition.
Wherein, the thermal conductivity of sintered aluminium nitride composite material reaches 175W/m K.
The technological merit of the present invention is：
1）The present invention selects aluminium nitride composite material to substitute magnesia as embedding packing material, and car tail temperature is improved with this
The thermal response time for spending sensor, can be promoted within 5 seconds.
2）Aluminium nitride composite material obtained by the present invention has high thermal conductivity, and is with suitable thermally expand
Number, and although aluminium nitride has very high thermal conductivity, aluminium nitride, which is added, can promote the thermal conductivity and thermal stability of system, but nitrogenize
Aluminium belongs to covalent compound, and self-diffusion coefficient is small, is excessively added, and sintering densification is extremely difficult.
3）Aluminium nitride composite material obtained by the present invention promotees as embedding packing material containing suitable sintering aid
Aluminium nitride molecular gap is melted and filled into silica in component, is improved the thermal conductivity of packing material, be ensure that car tail
The gas temperature sensor response time is the requirement within 5s.
Specific implementation mode：
With reference to embodiment, the present invention will be further described.
Embodiment 1
1）It weighs 70 parts of aluminium nitride micro mists, 25 parts of fine silica powders, 5 parts of aluminium oxide after mixing, 100 parts of anhydrous second is added
Alcohol, ball milling 1 hour, is made AlN- SiO in the ball mill2Matrix slurry；
2）By step 1）AlN-SiO obtained2Matrix slurry is dried 8 hours at 90 DEG C, is ground up, sieved 350 mesh, and drying is made
AlN-SiO2Matrix composite powder；
3）By step 2）AlN-SiO obtained2Composite material composite granule is packed into vehicle exhaust temperature sensor as filling
Closure material, 800 DEG C of sintering.
Embodiment 2
（1）Weigh 60 parts of aluminium nitride micro mists, 35 parts of fine silica powders, 5 parts of aluminium oxide after mixing, 100 parts of addition is anhydrous
Ethyl alcohol, ball milling 0.5 hour, is made AlN- SiO in the ball mill2Matrix slurry；
（2）By step 1）AlN-SiO obtained2Matrix slurry is dried 10 hours at 80 DEG C, is ground up, sieved 300 mesh, and drying is made
AlN-SiO2Matrix composite powder；
（3）By step 2）AlN-SiO obtained2Composite material mixed powder is packed into conduct in vehicle exhaust temperature sensor
Embedding Material, 600 DEG C of sintering.
Embodiment 3
1）It weighs 80 parts of aluminium nitride micro mists, 20 parts of fine silica powders after mixing, 100 parts of absolute ethyl alcohols is added, in ball milling
AlN- SiO are made in ball milling 2 hours in machine2Matrix slurry；
2）By step（1）AlN-SiO obtained2Matrix slurry is dried 6 hours at 100 DEG C, is ground up, sieved 300 mesh, and drying is made
AlN-SiO2Matrix mixed powder；
3）By step（2）AlN-SiO obtained2Composite material mixed powder is packed into conduct in vehicle exhaust temperature sensor
Embedding Material, 700 DEG C of sintering.
Embodiment 4
Sintering aid selects modified oxidized aluminium composite material, remaining is the same as embodiment 1.
The modified oxidized aluminium composite material is made by following preparation process：
（1）By 40 parts of aluminium oxide, 3 parts of nano zine oxide, 10 parts of silicon powder, 5 parts of magnesia, ball milling mixing is carried out, mixing is made
Slurry；Drum's speed of rotation is 250r/min, Ball-milling Time 2h, aluminium oxide, nano zine oxide, silicon powder, magnesia quality
The sum of mass volume ratio 1g with ball-milling medium：1mL, ball-milling medium are absolute ethyl alcohol-water-hydroxymethyl cellulose mixed solution,
Wherein absolute ethyl alcohol：Water：Hydroxymethyl cellulose presses mass volume ratio 1mL：1mL：2g is formulated；
（2）Mixed slurry obtained is first dried, then in 530 DEG C of sintering condition sintering temperature, sintering time 1 hour into
Row sintering, obtains modified oxidized aluminium composite material.
Embodiment 5
Sintering aid selects modified oxidized aluminium composite material, remaining is the same as embodiment 1.
The modified oxidized aluminium composite material is made by following preparation process：
（3）By 60 parts of aluminium oxide, 8 parts of nano zine oxide, 20 parts of silicon powder, 10 parts of magnesia, ball milling mixing is carried out, mixing is made
Slurry；Drum's speed of rotation is 200r/min, Ball-milling Time 2h, the aluminium oxide, nano zine oxide, silicon powder, magnesia
The mass volume ratio 1g of quality sum and ball-milling medium：5mL, ball-milling medium are that absolute ethyl alcohol-water-hydroxymethyl cellulose mixing is molten
Liquid, wherein absolute ethyl alcohol：Water：Hydroxymethyl cellulose presses mass volume ratio 1mL：1mL：2g is formulated；
（4）Mixed slurry obtained is first dried, then in 520 DEG C of sintering condition sintering temperature, sintering time 3 hours into
Row sintering, obtains modified oxidized aluminium composite material.
Embodiment 6
Sintering aid selects modified oxidized aluminium composite material, remaining is the same as embodiment 1.
The modified oxidized aluminium composite material is made by following preparation process：
By 50 parts of aluminium oxide, 5 parts of nano zine oxide, 15 parts of silicon powder, 8 parts of magnesia, ball milling mixing is carried out, mixing slurry is made
Material；Drum's speed of rotation is 250r/min, Ball-milling Time 1h, the aluminium oxide, nano zine oxide, silicon powder, magnesia matter
Mass volume ratio 1g of the sum of the amount with ball-milling medium：3mL, ball-milling medium are that absolute ethyl alcohol-water-hydroxymethyl cellulose mixing is molten
Liquid, wherein absolute ethyl alcohol：Water：Hydroxymethyl cellulose presses mass volume ratio 1mL：1mL：2g is formulated；
（5）Mixed slurry obtained is first dried, then in 520 DEG C of sintering condition sintering temperature, sintering time 3 hours into
Row sintering, obtains modified oxidized aluminium composite material.
After testing, sintered AlN- SiO in embodiment 1-32Heat conductivity about 150W/m K or so, heat are swollen
Swollen coefficient about 4.4 × 10-6DEG C, response time about 4.5s.Modified oxidized aluminium composite material is selected to be helped as sintering in embodiment 4-6
Agent, sintered AlN- SiO2Heat conductivity reaches 175W/m K or so, response time about 4.2s.
Claims (10)
1. a kind of aluminium nitride composite material, it is characterised in that：It is made of the material composition of following mass percent：Aluminium nitride 60~
80wt%, 20~35wt% of silica, 0~10 wt% of sintering aid, the sum of each Ingredient Amount are 100%.
2. aluminium nitride composite material according to claim 1, it is characterised in that：The sintering aid is aluminium oxide.
3. aluminium nitride composite material according to claim 1, it is characterised in that：The sintering aid is modified aluminas
Composite material.
4. aluminium nitride composite material according to claim 3, it is characterised in that：The modified oxidized aluminium composite material,
It is made from the following raw materials in parts by weight：40~60 parts of aluminium oxide, 3~8 parts of nano zine oxide, 10~20 parts of silicon powder, magnesia 5
~10 parts.
5. aluminium nitride composite material according to claim 4, it is characterised in that：The modified oxidized aluminium composite material by
Following preparation process is made：
In proportion by aluminium oxide, nano zine oxide, silicon powder, magnesia carry out ball milling mixing, drum's speed of rotation be 200~
250r/min, Ball-milling Time are 2~3h, and the ball-milling medium that ball milling is selected is that the mixing of absolute ethyl alcohol-water-hydroxymethyl cellulose is molten
Liquid, the aluminium oxide, nano zine oxide, silicon powder, the quality sum of magnesia and ball-milling medium mass volume ratio 1g：1~
5mL, the absolute ethyl alcohol-water-hydroxymethyl cellulose mixed solution press absolute ethyl alcohol：Water：Hydroxymethyl cellulose presses quality volume
Compare 1mL：1mL：2g is formulated, and mixed slurry is made；
2）By step 1）Mixed slurry obtained is first dried, and then re-sinters, and obtains modified oxidized aluminium composite material；It burns
Junction temperature is 520~530 DEG C, and sintering time is 1~3 hour.
6. a kind of method preparing the aluminium nitride composite material as described in any one of claims 1 to 3, it is characterised in that：Prepare step
Suddenly it is：
1）AlN-SiO2The preparation of matrix slurry；
Aluminium nitride, silica and sintering aid are uniformly mixed in proportion, absolute ethyl alcohol is added and carries out ball milling, AlN- is made
SiO2Matrix slurry；
2）AlN-SiO2The preparation of matrix composite powder；
By step 1）AlN-SiO obtained2The drying of matrix slurry grinds and is sieved, and AlN-SiO is made2Matrix composite powder.
7. a kind of preparation method of aluminium nitride composite material according to claim 6, it is characterised in that：Step 1）In, institute
The sum of aluminium nitride, silica and sintering aid weight for stating are 1 in mass ratio with absolute ethyl alcohol：1, Ball-milling Time is 0.5~2
Hour；Step 2）Described in drying temperature be 80~100 DEG C, drying time be 6~10 hours, sieving screening size be 300
~350 mesh.
8. a kind of method preparing aluminium nitride composite material as claimed in claim 4, it is characterised in that：Preparation process is：
1）The preparation of modified oxidized aluminium composite material
Aluminium oxide, nano zine oxide, silicon powder, magnesia are subjected to ball milling mixing in proportion, mill speed is 200~250r/
Min, Ball-milling Time are 2~3h, and the ball-milling medium that ball milling is selected is the mixed solution of absolute ethyl alcohol-water-hydroxymethyl cellulose, institute
State the mass volume ratio 1g of aluminium oxide, nano zine oxide, silicon powder, the quality sum of magnesia and ball-milling medium：1~10mL,
Mixed slurry is made；
Mixed slurry obtained is first dried, is then re-sintered, modified oxidized aluminium composite material is obtained；Sintering temperature is
520~530 DEG C, sintering time is 1~3 hour；
2）AlN-SiO2The preparation of matrix slurry；
In proportion by aluminium nitride, silica and step 1）Modified oxidized aluminium composite material obtained is uniformly mixed, and is added anhydrous
Ethyl alcohol carries out ball milling, and AlN- SiO are made2Matrix slurry；
3）AlN-SiO2The preparation of matrix composite powder；
Step 2 is added in epoxy resin and ethylenediamine in proportion）AlN-SiO obtained2In matrix slurry, normal temperature cure is carried out, Gu
It is 0.5~2 hour to change the time, is ground up, sieved after drying, and AlN-SiO is made2Matrix composite powder.
9. a kind of application of the aluminium nitride composite material in vehicle exhaust temperature sensor as described in any one of Claims 1 to 4,
It is characterized in that：Aluminium nitride composite material is packed into vehicle exhaust temperature sensor and is used as Embedding Material, and 600~
It is sintered under 800 DEG C of temperature condition.
10. a kind of application of the aluminium nitride composite material according to claim 9 in vehicle exhaust temperature sensor, special
Sign is：The thermal conductivity of sintered aluminium nitride composite material reaches 175W/m K.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149243A (en) * | 2021-12-21 | 2022-03-08 | 厦门钜瓷科技有限公司 | Inorganic encapsulating material, preparation method and application thereof, and temperature sensor |
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| JPH046162A (en) * | 1990-04-25 | 1992-01-10 | Nippon Steel Corp | Aln-bn-based composite sintered body and production thereof |
| WO2001023322A1 (en) * | 1999-09-28 | 2001-04-05 | 3M Innovative Properties Company | Method for making abrasive grain |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149243A (en) * | 2021-12-21 | 2022-03-08 | 厦门钜瓷科技有限公司 | Inorganic encapsulating material, preparation method and application thereof, and temperature sensor |
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