JP6284609B2 - Aluminum nitride sintered body - Google Patents

Description

  The present invention relates to an aluminum nitride sintered body and a method for producing the same.

  The aluminum nitride sintered product has excellent thermal conductivity and high electrical insulation, and has attracted attention as a material for high thermal conductivity substrates. The aluminum nitride sintered body is used for semiconductors and electronic devices whose operations are unstable due to high heat due to their excellent heat conduction characteristics. For example, power transistor module substrates, light-emitting diode mount substrates, IC packages, and other electronic components. Widely used as a heat dissipation board.

For example, Patent Document 1 discloses an aluminum nitride sintered body and a manufacturing method thereof. According to Patent Document 1, it is known that mechanical strength can be increased without impairing heat dissipation characteristics by variously changing the type and amount of the sintering aid and additive added to the raw aluminum nitride powder. Yes. For example, the sintering aid prevents densification of the sintered body and impurity oxygen in the aluminum nitride (AlN) raw material powder from forming a solid solution in the AlN crystal particles. Specific examples of the sintering agent include oxides of rare earth elements (Y, Sc, Ce, Dy, etc.), nitrides, oxides of alkaline earth metals (Ca, Sr, Ba), and the like. It is known that yttrium (Y ₂ O ₃ ), cerium oxide (CeO ₂ ), and calcium oxide (CaO) are preferable. Further, the Si component as an additive has the effect of improving the sinterability and lowering the sintering temperature. The Si component can be added in combination with a sintering aid to suppress the grain growth of the sintered body, to form a fine AlN crystal structure, and to increase the structural strength of the sintered body. It is known to be added. Further, it is known that the Hf compound and the Zr compound have the effect of further improving the sinterability and suppressing the aggregation and segregation of the liquid phase that is likely to occur on the surface of the sintered body and expanding the temperature range in which the sintering can be properly performed. It has been.

JP 2003-201179 A

  Aluminum nitride sintered substrates are often used for semiconductor circuit boards used in power modules and the like. In recent years, the amount of heat generated per unit area tends to increase due to higher output and smaller size of modules. For this reason, the ceramic insulating substrate is required to have higher strength as well as high heat dissipation. For example, the aluminum nitride sintered body of Patent Document 1 (for example, Example 15 of Patent Document 1) has high thermal conductivity, but further improves the strength while maintaining this thermal conductivity. Is desirable. And although the compositional approach like patent document 1 has done many experiment and research in the past, improving the characteristic of an aluminum nitride sintered compact by reviewing a manufacturing process is not paid much attention. For example, in a conventional manufacturing process such as Patent Document 1, an aluminum nitride raw material powder, a powdered silicon compound, a sintering aid, and an additive are charged into a ball mill at a time, and pulverized and mixed in the ball mill. This invention pays attention to the raw material mixing process of the aluminum nitride sintered compact, and improves the characteristic.

  The present invention has been made to solve the above-described problems, and an object of the present invention is to provide an aluminum nitride sintered body having higher strength while maintaining at least thermal conductivity, and a method for producing the same. .

The method for producing the aluminum nitride sintered body of the present invention is as follows.
A primary mixing step of mixing at least two of a silicon compound, a sintering aid, and an additive to produce a primary mixture;
A secondary mixing step of preparing the raw material mixture by mixing the primary mixture with the aluminum nitride raw material powder;
Forming the raw material mixture and firing in a predetermined temperature range;
It is characterized by including.

The aluminum nitride sintered body of the present invention is 0.025 to 0.15 parts by weight of SiO _{2 in} terms of Si element and 1 to 10 parts by weight of Y in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder. A molded body of a raw material mixture containing ₂ O ₃ and 1 to 10 parts by weight of partially stabilized zirconia in terms of oxide is fired.

The aluminum nitride sintered body of the present invention is 0.025 to 0.15 parts by weight of SiO _{2 in} terms of Si element and 1 to 10 parts by weight of Y in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder. ₂ O ₃ and an aluminum nitride sintered body obtained by firing a molded body of a raw material mixture containing 0.5 to 5 parts by weight of partially stabilized zirconia in terms of oxide, wherein the ZrN particles are in the range of 0. 4 to 4.2 wt% is precipitated.

  The method for producing an aluminum nitride sintered body of the present invention introduces a primary mixing step in which a silicon compound, a sintering aid, and an additive are mixed to produce a primary mixture, compared to the conventional raw material mixing step. Features. And by introducing the above-mentioned process, at least as compared with the conventional aluminum nitride sintered body in which the aluminum nitride raw material powder, the powdered silicon compound, the sintering aid and the additive are added at once and mixed. The knowledge that the strength (three-point bending strength) was improved while maintaining the thermal conductivity was obtained. That is, a primary mixture in which the raw materials are dispersed with each other by mixing the silicon compound, the sintering aid, and the additive in advance before blending into the relatively high weight aluminum nitride raw material powder in the primary mixing step. Is formed. And the dispersibility of each raw material can be relatively improved by mixing the aluminum nitride raw material powder with the primary mixture in which the silicon compound, the sintering aid and the additive are sufficiently dispersed. This makes it possible to produce a raw material mixture in which the particles of each raw material are more uniformly dispersed in the aluminum nitride raw material powder. As a result, the strength of the aluminum nitride sintered body can be relatively improved without changing the material composition.

The scanning electron microscope (SEM) image which shows the crystal structure of the aluminum nitride sintered compact of a prior art example (comparative example). The EDX analysis image which shows Zr element distribution in the aluminum nitride sintered compact of a prior art example (comparative example). The scanning electron microscope (SEM) image which shows the crystal structure of the aluminum nitride sintered compact of one Embodiment (Example 4) of this invention. The EDX analysis image which shows Zr element distribution in the aluminum nitride sintered compact of one Embodiment (Example 4) of this invention.

  The aluminum nitride sintered body substrate of the present embodiment includes a first step of preparing an aluminum nitride raw material powder, a silicon compound, a sintering aid and an additive, and nitriding a predetermined amount of the silicon compound, the sintering aid and the additive. It is manufactured through a second step in which a raw material mixture is prepared by mixing with aluminum raw material powder and a third step in which the raw material mixture is formed and fired in a predetermined temperature range.

In this embodiment, the silicon compound is SiO ₂ fine particles having a particle diameter of 10 to 15 nm. However, the particle size of the silicon compound can be arbitrarily changed as long as it can be dispersed in a solvent. The fine particles of SiO ₂ preferably have a particle diameter of 10 nm to 100 nm as a range that can be stably dispersed in a solvent. And the density | concentration of the silica solid content of the silica sol of this embodiment is 30%. However, the concentration can be arbitrarily changed if it does not aggregate or settle upon addition.

  The dispersion solvent of the silicon compound is preferably one kind selected from ethanol, isopropyl alcohol or toluene or a mixture thereof. However, the present invention is not limited to the above solvents, and examples thereof include methanol, dimethylacetamide, ethylene glycol, ethylene glycol mono n-propyl ether (NPG), propylene glycol monomethyl ether (PGM), ethyl acetate (EAC), and propylene glycol monomethyl. It may be at least one selected from the group consisting of ether acetate (PMA), methyl ethyl ketone (MEK) and methyl isobutyl ketone.

Further, the silicon compound may be at least one selected from the group consisting of SiO ₂ , amorphous SiO ₂ , and a hydrolyzate of silicon alkoxide.

  That is, in the colloidal silicon compound, the particle diameter, particle shape, liquidity, viscosity, and type of dispersion solvent can be arbitrarily selected.

  Next, 100 parts by weight of the aluminum nitride raw material powder is determined, the weight part of Si to be added in terms of Si is determined, and the amount of colloidal silicon compound added as the Si source is calculated based on the weight part.

Then, an appropriate amount of sintering aid powder and an appropriate amount of additive powder are prepared together with an appropriate amount of aluminum nitride raw material powder. The aluminum nitride raw material powder is preferably a high-purity fine powder with few metal impurities and low oxygen content. The sintering aid is at least one selected from the group consisting of Y ₂ O ₃ , Yb ₂ O ₃ , and CaO. As the additive, ZrO ₂ or partially stabilized zirconia is used. The additive is preferably partially stabilized zirconia (PSZ). It has been found that the addition of partially stabilized zirconia improves the strength compared to the usual addition of ZrO ₂ . These sintering aids and additives are added in terms of oxides with 100 parts by weight of the aluminum nitride raw material powder. The oxide may be added in the form of nitride or the like.

  Subsequently, in the second step, a silicon compound, a sintering aid and an additive are mixed with the aluminum nitride raw material powder to produce a raw material mixture. The second step includes a primary mixing step of preparing a primary mixture by mixing a silicon compound (preferably silica sol), a sintering aid, and an additive, and mixing (or grinding and mixing) the primary mixture with the aluminum nitride raw material powder. ) To prepare a raw material mixture. In this mixing step (primary and secondary mixing step), for example, each material is put into a pulverizing mixer such as a ball mill, and an organic solvent, a dispersant and / or an organic binder are arbitrarily added, and a predetermined time is taken. The mixed material is ground and mixed.

  In the primary mixing step, a predetermined amount of an organic solvent and a dispersant are added to the mixed material of the silicon compound (silica sol), the sintering aid, and the additive, and the mixed material is pulverized and mixed for the first mixing time. The organic solvent is, for example, a solvent prepared by mixing toluene, ethanol, and butanol at a predetermined ratio. The amount of the organic solvent is about 10 to 20 parts by weight with 100 parts by weight of the aluminum nitride raw material powder. Moreover, a dispersing agent is a trace amount phosphorus type surfactant, for example. However, these organic solvents and dispersants can be arbitrarily selected.

  Although this 1st mixing time changes with the capability of the mixer to be used, suitable mixing time changes, It is preferable that it is about 0.5 to 3 hours. When the first mixing time is less than 0.5 hours, the dispersion and mixing of each raw material in the primary mixture is insufficient, and an aluminum nitride sintered body having desired characteristics cannot be obtained. On the other hand, if the primary mixing time is longer than 3 hours, the particles of each raw material are excessively pulverized, and similarly, an aluminum nitride sintered body having desired characteristics cannot be obtained.

  And after a primary mixture is obtained, a predetermined amount of aluminum nitride raw material powder is thrown into a ball mill, and a secondary mixing process is performed. The secondary mixing step includes a first stage in which a predetermined amount of an organic solvent is added and the primary mixture and the aluminum nitride raw material powder are mixed over a second mixing time, and a predetermined amount of the mixed material mixed in the first stage. And adding a binder and a plasticizer, and mixing the primary mixture and the aluminum nitride raw material powder over a third mixing time.

  In the first stage, the organic solvent is a solvent prepared by mixing, for example, toluene and ethanol at a predetermined ratio. The amount of the organic solvent is about 10 to 20 parts by weight with 100 parts by weight of the aluminum nitride raw material powder. The second mixing time is preferably 12 to 24 hours.

  In the second stage, the organic solvent is a solvent in which, for example, toluene and ethanol are added at a predetermined ratio. The additional amount of the organic solvent is about 10 to 15 parts by weight with 100 parts by weight of the aluminum nitride raw material powder. In addition, for example, polyvinyl butyral resin (BM-S manufactured by Sekisui Chemical Co., Ltd.) is used as the binder. The amount added is about 5 to 10 parts by weight with 100 parts by weight of the aluminum nitride raw material powder. For example, dibutyl phthalate (DBP) is used as the plasticizer. The addition amount is about 1 to 5 parts by weight with 100 parts by weight of the aluminum nitride raw material powder. And it is preferable that 3rd mixing time is 12 to 24 hours. These binders and plasticizers can be arbitrarily selected as long as they have similar actions or properties.

  By the second step as described above, a slurry-like raw material mixture in which the raw materials are sufficiently dispersed and mixed is obtained. Then, in the third step, the obtained raw material mixture is formed into a predetermined shape by means of an extrusion molding method, a casting molding method, a doctor blade molding method, or the like.

  The molded body thus molded is heated to 400 to 800 ° C. in vacuum or in a non-oxidizing atmosphere (for example, nitrogen gas), and the binder added over 5 to 10 hours is degreased and removed. The degreased compact is fired at 1700 to 1800 ° C. for 3 to 10 hours in a nitrogen gas atmosphere. At this time, since the Si component is added, sintering can be performed at a relatively low temperature of about 1700 ° C. In this way, a substrate of aluminum nitride sintered body is obtained.

  Then, the characteristics of the aluminum nitride sintered body were evaluated by measuring the thermal conductivity, bending strength, crystal phase identification by X-ray diffraction, and microstructure observation of the aluminum nitride sintered body.

  EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example and a comparative example, this invention is not limitedly interpreted by the following Example.

  The aluminum nitride sintered bodies according to Examples 1 to 24 were produced by performing part or all of the following procedures.

(1) A predetermined amount of aluminum nitride raw material powder was prepared. The aluminum nitride raw material powder having an average particle size of about 1.1 μm and a specific surface area of 2.6 m ² / g was employed. (Examples 1 to 24)

(2) A predetermined amount of silica sol was prepared as a colloidal silicon compound. An appropriate amount of silica sol was prepared based on an addition amount in terms of Si element with 100 parts by weight of the aluminum nitride raw material powder. The silica sol is a fine particle of SiO _{2 having} a particle diameter of 10 to 15 nm, a dispersion solvent is IPA, and a dispersion having a silica solid content concentration of 30% (organosilica sol manufactured by Nissan Chemical Industries, Ltd.) is used. did. (Examples 8 to 22)
On the other hand, in Example 23, silica powder having a purity of 99.8% and a particle size of 1.2 μm was prepared as a Si source.

(3) A high purity yttrium oxide (Y ₂ O ₃ ) powder was prepared as a sintering aid. The addition amount of the sintering aid is preferably 1 to 10 parts by weight. In this example, in order to understand the effect of the additive more accurately, all of them were set to 5 parts by weight. (Examples 1 to 24)

(4) As optional additives, ZrO ₂ powder and partially stabilized zirconia (PSZ) powder were prepared. As the partially stabilized zirconia, a material in which 2 to 4 mol% of Y ₂ O ₃ is dissolved in ZrO ₂ is preferably used. In this example, a raw material in which 3 mol% is dissolved is used. Since Y ₂ O _{3 in} PSZ is extremely small compared to the weight of AlN, it can be ignored. (Examples 1-7, 13-22, 24)

(5) A raw material composition was prepared by adding an appropriate amount of each raw material to 100 parts by weight of the aluminum nitride raw material powder. (Examples 1 to 24)

(6) Each raw material was charged stepwise into the ball mill, and the primary mixing step and the secondary mixing step (first step and second step) were performed under the conditions shown in Table 1. (Examples 1 to 24)

(7) The raw material mixture was formed into a sheet by the doctor blade method and formed into a desired shape by a mold (punching). (Examples 1 to 24)

(8) A sheet molded body of the raw material mixture is coated with powder, laminated, degreased by heating at 550 ° C. for 7 hours in a vacuum, and subsequently, 1700 to 1800 ° C. for 5 hours in a nitrogen gas atmosphere. And then baked. (Examples 1 to 24)

  The aluminum nitride sintered body according to Comparative Example 1 is obtained by omitting the primary mixing step of Table 1 and performing only the secondary mixing step (first stage, second stage). The other steps are the same as in the method for manufacturing the aluminum nitride sintered body according to Example 4.

  Regarding the aluminum nitride sintered bodies of Examples 1 to 24 and Comparative Example 1, characteristics A to C were evaluated by the following method.

A. Bending strength A three-point bending test was adopted as a measuring method for measuring bending strength. As the aluminum nitride sintered body for evaluation, a test piece of 63 mm × 20 mm × 0.32 mmt was used. The measuring device was model AG-IS manufactured by Shimadzu Corporation, and the measurement conditions were set to 20 pcs, the crosshead speed was 0.5 mm / min, and the distance between fulcrums was 30 mm, and the average value was obtained.

B. Thermal conductivity The laser flash method was adopted as a method for measuring thermal conductivity. As the test piece of the aluminum nitride sintered body, a test piece having a size of 25 mm × 25 mm was used. The measuring device was model TC-7000 manufactured by ULVAC-RIKO, and the measurement condition was set to 2 pcs and the average value was obtained.

C. Crystal phase identification (ZrN production)
An X-ray diffraction method using Cu-Kα rays was employed for crystal phase identification. The aluminum nitride sintered body was pulverized with a mortar, embedded in a holder having a size of 10 mm × 10 mm, and measured. The amount of ZrN produced was calculated by the WPPF method based on the peak intensity (area) detected by the measured X-ray diffraction. The measuring device was a model Ultima IV manufactured by Rigaku Corporation, and the number of measurements was 1 pcs.

The characteristics A to C (measurement results) of the aluminum nitride sintered body of each example are shown in Table 2 below. The blending amount of the raw material mixture is 100 parts by weight of the aluminum nitride raw material powder (AlN), the weight part of Y ₂ O ₃ converted to oxide, the weight part of ZrO ₂ converted to oxide, and the Si element It was shown as parts by weight of the converted silicon compound.

In Example 4, 5 parts by weight of Y ₂ O ₃ and 2 parts by weight of ZrO ₂ were added to 100 parts by weight of AlN. And Example 4 (with a primary mixing process) and Comparative Example 1 (without a primary mixing process) are the same in terms of the blending amount, but differ in the presence or absence of a primary mixing process. In Example 4, the strength is 580 MPa and the thermal conductivity is 149 W / mK, whereas in the comparative example, the strength is 493 MPa and the thermal conductivity is 150 W / mK. That is, in Example 4, compared with the comparative example, the strength of about 90 MPa (about 18%) is improved while maintaining the thermal conductivity. Therefore, it was confirmed that the strength was improved without lowering the thermal conductivity by introducing the primary mixing step.

Further, Example 4 (PSZ as an additive) and Example 24 (ZrO ₂ as an additive) are the same in terms of blending amount, but Y ₂ dissolved in ZrO ₂ used as an additive. The difference is in the presence or absence of O ₃ . In Example 4, the strength is 580 MPa and the thermal conductivity is 149 W / mK, whereas in Example 24, the strength is 507 MPa and the thermal conductivity is 148 W / mK. That is, in Example 4, compared with Example 24, the strength of about 73 MPa (about 14%) is improved while maintaining the thermal conductivity. Therefore, it was confirmed that the use of partially stabilized zirconia (PSZ) as an additive improves the strength without lowering the thermal conductivity.

  FIG. 1 shows the result of surface observation (magnification 8000) by SEM of the aluminum nitride sintered body according to Comparative Example 1, and FIG. 2 shows the analysis result in EDX (energy dispersive X-ray spectroscopy) (the bright spot is Zr). Element). The surface analysis and EDX analysis were performed with model S-3400N manufactured by Hitachi High-Technologies Corporation. FIG. 3 shows the result of surface observation (magnification 8000) by SEM of the aluminum nitride sintered body according to Example 4. FIG. 4 shows an analysis result (bright spot is Zr element) in EDX (energy dispersive X-ray spectroscopy). In the SEM images of FIGS. 1 and 3, it is found by crystal phase identification by X-ray diffraction and EDX analysis that the particles or lumps indicated by arrows are ZrN.

  1 and 2, it can be seen that in the comparative aluminum nitride sintered body produced by the conventional manufacturing method, ZrN does not uniformly disperse and exists as a large lump of 1.5 μm or more. On the other hand, according to FIG. 3 and FIG. 4, in the aluminum nitride sintered body (Example 4) into which the primary mixing step was introduced, ZrN was uniformly dispersed as fine particles as compared with the comparative example, and the particle size Is found to be about 0.1 to 0.8 μm. Further, according to the SEM image, in the comparative example of FIG. 1, due to the presence of the ZrN lump, the AlN particles are partially separated (variation in grain boundaries), and the AlN crystal particles are messy as a whole. On the other hand, in Example 4 of FIG. 3, since the ZrN fine particles are uniformly dispersed, the grain boundaries between the AlN grains are narrow, the widths of the grain boundaries are almost uniform, and the AlN crystal grains are They are regularly arranged as a whole. That is, as shown in FIGS. 1 to 4, the introduction of the primary mixing step causes a noticeable structural change in the resultant product (aluminum nitride sintered body). As a result, it was found that the strength of the aluminum nitride sintered body was greatly improved.

However, the principle of the phenomenon that the dispersion of ZrN contributes to the improvement of the strength of the aluminum nitride sintered body has not yet been elucidated.

Examples 1 to 7, without the addition of _Si, is obtained by changing the ZrO 2 (PSZ) amount. As shown in Table 2, with respect to 100 parts by weight of AlN, when the ZrO ₂ content is 0.5 to 5 parts by weight (Examples 4 and 5), the three-point bending strength is 550 MPa or more, and heat Conductivity is 130 W / mK or more. And, as in Examples 6 and 7, when the amount of ZrO ₂ exceeds 5 parts by weight, the strength increases, but the thermal conductivity decreases remarkably. That is, according to Table 2, it is preferable that the compounding quantity of Zr is 0.5-5 weight part in conversion of an oxide.

In Examples 8 to 12, the compounding amount of Si (silica sol) was changed without adding ZrO ₂ . As shown in Table 2, with respect to 100 parts by weight of AlN, when the Si compounding amount is 0.025 to 0.2 parts by weight (Examples 8 to 11) in terms of Si element, the three-point bending strength is 540 MPa or more. And the thermal conductivity is 140 MPa or more. And like Example 12, when Si compounding quantity will be 0.5 weight part, the fall of intensity | strength will become remarkable. That is, according to Table 2, the Si compounding amount is preferably 0.025 to 0.2 parts by weight.

In Example 10, 5 parts by weight of Y ₂ O ₃ and 0.1 part by weight of silica sol (colloidal silicon compound) in terms of Si element are added to 100 parts by weight of AlN. In contrast, in Example 23, 5 parts by weight of Y ₂ O ₃ and 0.1 parts by weight of silica powder in terms of Si element are added to 100 parts by weight of AlN. That is, Example 12 and Example 23 differ in the state of Si to be added (mixed). In Example 10, the strength is 600 MPa and the thermal conductivity is 143 W / mK, whereas in Example 23, the strength is 520 MPa and the thermal conductivity is 127 W / mK. . That is, in Example 10, compared with Example 22, the strength of about 80 Mpa (about 15%) is improved, and the thermal conductivity of about 16 W / mK (about 13%) is improved. Therefore, it was confirmed that the strength and thermal conductivity were improved by employing silica sol instead of silica powder.

In Examples 13 to 22, the amount of partially stabilized zirconia and / or Si (silica sol) is changed. In particular, the aluminum nitride sintered bodies according to Examples 13 to 22 have a three-point bending strength of 650 MPa or more and a thermal conductivity of 130 W / m · K or more, and have extremely good characteristics. That is, in the raw material mixture of the aluminum nitride sintered body, 5 parts by weight of Y ₂ O ₃ , 0.5 to 5 parts by weight of ZrO ₂ , and 0.025 to 0.15 parts by weight with respect to 100 parts by weight of AlN. The amount of Si is suitable in view of characteristics.

  Examples 2-7, 13-22, and 24 deposit ZrN. In particular, the aluminum nitride sintered bodies according to Examples 13 to 22 have a three-point bending strength of 650 MPa or more and a thermal conductivity of 130 W / m · K or more, and have good characteristics. That is, it was confirmed that suitable strength and thermal conductivity can be obtained by depositing 0.4% to 4.2 wt% of ZrN in the aluminum nitride sintered body.

Further, among these, the aluminum nitride sintered bodies according to Examples 15, 17, 19, and 20 exhibit a three-point bending strength of 660 MPa or more and a thermal conductivity of 140 W / m · K or more, and have extremely good characteristics. Have. That is, in the raw material mixture of the aluminum nitride sintered body, 1 to 10 parts by weight of Y ₂ O ₃ , 2 to 3 parts by weight of partially stabilized zirconia, and 0.05 parts by weight with respect to 100 parts by weight of the aluminum nitride raw material powder It is the compounding amount of Si of ~ 0.1 part by weight, and 1.4 to 2.5 wt% of ZrN particles are precipitated in the aluminum nitride sintered body, so that the most suitable strength and heat conduction in terms of properties. It was confirmed that the rate was obtained.

  According to the aluminum nitride sintered body and its manufacturing method of the present embodiment (Examples 1 to 24), the introduction of the primary mixing step has the same composition as that of the aluminum nitride sintered body that does not introduce the above steps. The improvement of relative strength is realized.

  In addition, regarding elements and components not included in the above-described examples, if the same properties as sintering aids and additives are obtained, it is possible to benefit from the production method of the present invention. Any substitution, omission and / or addition can be made within the technical scope of (1).

The present invention is not limited to the above-described embodiments and modifications, and can be implemented in various modes as long as they belong to the technical scope of the present invention.
(Additional remark) This specification discloses the following structures.
Configuration 1. 0.025 to 0.15 parts by weight of SiO2 in terms of Si, 1 to 10 parts by weight of Y2O3 in terms of oxide, and 1 to 5 parts by weight in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder An aluminum nitride sintered body that is a sintered body of a molded body of a raw material mixture containing partially stabilized zirconia.
Configuration 2. 0.025 to 0.15 parts by weight of SiO2 in terms of Si, 1 to 10 parts by weight of Y2O3 in terms of oxide, and 1 to 5 parts by weight in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder An aluminum nitride sintered body characterized in that 0.7 to 4.2 wt% of ZrN particles are precipitated.
Configuration 3. The aluminum nitride sintered body according to Configuration 2, wherein the ZrN particles are uniformly dispersed and precipitated.
Configuration 4. 4. The aluminum nitride sintered body according to Structure 2 or 3, wherein the ZrN particles have an average particle diameter of 0.1 to 0.8 μm.
Configuration 5. The aluminum nitride sintered body according to any one of configurations 1 to 4, wherein the thermal conductivity is 130 W / m · K or more and the three-point bending strength is 650 MPa or more.
Configuration 6. With respect to 100 parts by weight of the aluminum nitride raw material powder, 0.05 to 0.1 parts by weight of SiO 2 in terms of Si element, 1 to 10 parts by weight of Y 2 O 3 in terms of oxide, and 2 to 3 parts by weight in terms of oxide A sintered body of a molded body of a raw material mixture containing ZrN particles of 1.4 to 2.5 wt% and a thermal conductivity of 140 W / m · K or more. An aluminum nitride sintered body having a three-point bending strength of 660 MPa or more.
Configuration 7. A primary mixing step of mixing a silicon compound and a sintering aid to produce a primary mixture;
A secondary mixing step of preparing the raw material mixture by mixing the primary mixture with the aluminum nitride raw material powder;
Forming the raw material mixture and firing in a predetermined temperature range;
Including
The raw material mixture contains 0.025 to 0.2 parts by weight of SiO2 in terms of Si element and 1 to 10 parts by weight of Y2O3 in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder. A manufacturing method of a featured aluminum nitride sintered body.

Claims (5)

0.025 to 0.15 parts by weight of SiO _{2 in} terms of Si element, 1 to 10 parts by weight of Y ₂ O _{3 in} terms of oxide, and 1 in terms of oxide with respect to 100 parts by weight of the aluminum nitride raw material powder. A sintered body of a compact of a raw material mixture containing ˜5 parts by weight of partially stabilized zirconia, wherein ZrN particles are precipitated in an amount of 0.7 to 4.2 wt%, and the thermal conductivity is 130 W / m · K or more. And a three-point bending strength of 650 MPa or more . The aluminum nitride sintered body according to claim 1 , wherein the ZrN particles are uniformly dispersed and precipitated. The aluminum nitride sintered body according to claim 1 or 2 , wherein an average particle diameter of the ZrN particles is 0.1 to 0.8 µm. With respect to 100 parts by weight of the aluminum nitride raw material powder, 0.05 to 0.1 parts by weight of SiO _{2 in} terms of Si element, 1 to 10 parts by weight of Y ₂ O _{3 in} terms of oxide, and 2 in terms of oxide. A sintered compact of a molded body of a raw material mixture containing ~ 3 parts by weight of partially stabilized zirconia, with 1.4 to 2.5 wt% of ZrN particles precipitated and a thermal conductivity of 140 W / m An aluminum nitride sintered body characterized by being K or higher and having a three-point bending strength of 660 MPa or higher. SiO ₂ Is contained in the raw material mixture as a silica sol, The aluminum nitride sintered body according to any one of claims 1 to 4.