TWI728073B - Pollinite sintered body, its manufacturing method and composite substrate - Google Patents
Pollinite sintered body, its manufacturing method and composite substrate Download PDFInfo
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 28
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 7
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- 239000002994 raw material Substances 0.000 claims description 40
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- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 6
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- 244000225942 Viola tricolor Species 0.000 claims description 2
- 235000004031 Viola x wittrockiana Nutrition 0.000 claims description 2
- 240000006240 Linum usitatissimum Species 0.000 claims 1
- 235000004431 Linum usitatissimum Nutrition 0.000 claims 1
- 238000005245 sintering Methods 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
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Abstract
本發明之菫青石質燒結體以菫青石為主成分、包含氮化矽或碳化矽。此菫青石質燒結體較佳40~400℃熱膨脹係數為未滿2.4ppm/℃,開氣孔率為0.5%以下,平均結晶粒徑為1μm以下。 The sintered sintered body of flatilite of the present invention is mainly composed of flatilite and contains silicon nitride or silicon carbide. It is preferable that the sintered body made of flatilite has a thermal expansion coefficient of less than 2.4 ppm/°C at 40 to 400°C, an open porosity of 0.5% or less, and an average crystal grain size of 1 μm or less.
Description
本發明係有關於菫青石質燒結體、其製法及複合基板。 The present invention relates to a sintered body of calalite, its preparation method and a composite substrate.
菫青石已知為耐熱性高、熱膨脹係數小的材料,可作為熱衝擊性高的材料。為了使菫青石的機械特性向上,菫青石中也已知可與楊氏模數或強度高的氮化矽或碳化矽等複合(專利文獻1、2)。專利文獻1揭露,於平均粒徑1.2μm的菫青石中添加稀土類氧化物及氮化矽或碳化矽,在大氣中進行燒成,以獲得相對密度97~98%的菫青石質燒結體。專利文獻2揭露,於平均粒徑3μm的菫青石中添加平均粒徑1μm的氮化矽或碳化矽,在氮氣環境中進行常壓燒成,以獲得楊氏模數高的菫青石質燒結體。
Pollinite is known as a material with high heat resistance and a small coefficient of thermal expansion, and can be used as a material with high thermal shock resistance. In order to improve the mechanical properties of flatidite, it is also known that flatidite can be combined with silicon nitride or silicon carbide with high Young's modulus or strength (Patent Documents 1 and 2). Patent Document 1 discloses that rare earth oxides and silicon nitride or silicon carbide are added to a vermilionite with an average particle diameter of 1.2 μm and fired in the air to obtain a vermilionite sintered body with a relative density of 97 to 98%.
此外,專利文獻3揭露,將鉭酸鋰或鈮酸鋰等所構成的機能性基板與菫青石燒結體製的支持基板直接接合所形成的複合基板,作為彈性表面波元件等彈性波元件。此彈性波元件中,由於支持基板之菫青石燒結體的熱膨脹係數為非常小的1.1ppm/℃(40-400℃),所以頻率溫度依賴性被大幅改善。
In addition,
【先前技術文獻】 【Prior Technical Literature】
【專利文獻】 【Patent Literature】
專利文獻1:專利第3574560號公報 Patent Document 1: Patent No. 3574560
專利文獻2:專利第4416191號公報 Patent Document 2: Patent No. 4416191
專利文獻3:國際專利公開第2015/186571號 Patent Document 3: International Patent Publication No. 2015/186571
以專利文獻3的方式接合機能性基板與支持基板時,兩基板的表面被要求具有高度平坦性。然而,專利文獻1之菫青石質燒結體的相對密度為97~98%,且存在數個百分比的氣孔,即使對燒結體的表面進行研磨加工,也無法獲得高平坦性。此外,專利文獻2的菫青石質燒結體,其菫青石原料粒子為3μm,且添加助燒結劑,導致燒結粒徑變得比菫青石原料粒子大。因此,即使進行研磨加工,也無法獲得高度的平坦性。此外,若將此菫青石質燒結體作為彈性波元件時,燒結粒徑也變得大於電極之間的間隔,此時可能會產生複合基板的音速變化,造成元件特性的改變。
When a functional substrate and a supporting substrate are joined in the manner of
為解決上述問題,本發明主要目的係為使菫青石質燒結體可維持菫青石的低熱膨脹係數,提高剛性以及增加研磨面的平坦性。 In order to solve the above-mentioned problems, the main purpose of the present invention is to maintain the low thermal expansion coefficient of the flatilite sintered body, improve the rigidity and increase the flatness of the polishing surface.
本發明菫青石質燒結體係為一種以菫青石為主成份,包含氮化矽或碳化矽的菫青石質燒結體,40~400℃熱膨脹係數為未滿2.4ppm/℃,開氣孔率為0.5%以下,平均結晶粒徑(燒結粒子的平均粒徑)為1μm以下。若使用此菫青石質燒結 體,可維持菫青石的低熱膨脹係數,提高剛性以及增加研磨面的平坦性。 The sintering system of plastolite of the present invention is a sintered body of plastolite containing silicon nitride or silicon carbide, which is mainly composed of plastinite, and has a thermal expansion coefficient of less than 2.4ppm/°C at 40~400°C and an open porosity of 0.5%. Hereinafter, the average crystal particle diameter (average particle diameter of sintered particles) is 1 μm or less. If you use this sintered glazeite Body, can maintain the low thermal expansion coefficient of the flatilite, improve the rigidity and increase the flatness of the polishing surface.
本發明菫青石質燒結體的製法包括(a)將60~90體積%平均粒徑0.1~1μm的菫青石粉末與10~40%體積%平均粒徑0.1~1μm的氮化矽粉末混合,合計100體積%,以獲得混合原料粉末,或將70~90體積%平均粒徑0.1~1μm的菫青石粉末與10~30體積%平均粒徑0.1~1μm的碳化矽粉末混合,合計100體積%,以獲得混合原料粉末的步驟;以及(b)將上述混合原料粉末形成所定形狀的成形體,此成形體以20~300kgf/cm2壓力、1350~1450℃燒成溫度(最高溫度)進行熱壓燒成,以獲得菫青石質燒結體的步驟。此製法適合用於製造本發明菫青石質燒結體。此外,粉末的平均粒徑以雷射繞射法測定(以下相同)。 The method for preparing the flatilite sintered body of the present invention includes (a) mixing 60 to 90% by volume of flatilite powder with an average particle size of 0.1 to 1 μm and 10 to 40% by volume of silicon nitride powder with an average particle size of 0.1 to 1 μm. 100% by volume to obtain mixed raw material powder, or mix 70~90% by volume of vermilionite powder with an average particle size of 0.1~1μm and 10-30% by volume of silicon carbide powder with an average particle size of 0.1~1μm, totaling 100% by volume, The step of obtaining mixed raw material powder; and (b) forming the above-mentioned mixed raw material powder into a shaped body of a predetermined shape, which is hot-pressed at a pressure of 20 to 300 kgf/cm 2 and a sintering temperature of 1350 to 1450°C (maximum temperature) The step of firing to obtain a sintered body of vermilionite. This production method is suitable for the production of the sintered sintered body of vermilionite of the present invention. In addition, the average particle size of the powder was measured by the laser diffraction method (the same applies below).
本發明之複合基板為接合機能性基板與支持基板的複合基板,此支持基板為上述菫青石質燒結體。由於此複合基板中作為支持基板之菫青石質燒結體的研磨面平坦性高,可與機能性基板良好地接合。此外,於彈性表面波元件中使用此複合基板時,可大幅地改善頻率溫度依賴性。再者,即使在光導波元件、LED元件、開關元件中,因支持基板的熱膨脹係數小,可提升性能。 The composite substrate of the present invention is a composite substrate in which a functional substrate and a support substrate are joined, and the support substrate is the above-mentioned sintered body of calalite. Since the polished surface of this composite substrate, which is a support substrate, of the sintered sintered vermilionite has high flatness, it can be well bonded to a functional substrate. In addition, when this composite substrate is used in a surface acoustic wave device, the frequency-temperature dependence can be greatly improved. Furthermore, even in optical waveguide elements, LED elements, and switching elements, the support substrate has a small coefficient of thermal expansion, so performance can be improved.
10‧‧‧複合基板 10‧‧‧Composite substrate
12‧‧‧壓電基板 12‧‧‧Piezoelectric substrate
14‧‧‧支持基板 14‧‧‧Support substrate
30‧‧‧電子元件 30‧‧‧Electronic components
32、34‧‧‧IDT電極 32、34‧‧‧IDT electrode
36‧‧‧反射電極 36‧‧‧Reflective electrode
第1圖為菫青石質燒結體的製造工程圖。 The first figure is the manufacturing process drawing of the sintered body of flatilite.
第2圖為複合基板10的斜視圖。
FIG. 2 is a perspective view of the
第3圖為使用複合基板10所製作之電子元件30的斜視圖。
FIG. 3 is a perspective view of the
第4圖為實驗例3菫青石質燒結體研磨面的SEM影像,(a)原始數據,(b)二值化處理後的數據。 Fig. 4 is an SEM image of the polished surface of the sintered body of vermilionite in Experimental Example 3, (a) the original data, and (b) the data after the binarization process.
以下,對本發明的實施形態進行說明,但不可用於限定本發明,在不偏離隨附權利要求書所界定的本發明的精神與範圍下,所屬本領域技術人員當可基於通常知識進行各種改變、改良。 The following describes the embodiments of the present invention, but they cannot be used to limit the present invention. Without departing from the spirit and scope of the present invention defined by the appended claims, those skilled in the art can make various changes based on common knowledge. , Improve.
本實施形態的菫青石質燒結體係以菫青石為主成份,包含氮化矽或碳化矽。主成份係指燒結體中含有最大體積的成份。此菫青石質燒結體較佳40~400℃熱膨脹係數為未滿2.4ppm/℃,開氣孔率為0.5%以下,平均結晶粒徑為1μm以下。此菫青石質燒結體雖然含有比菫青石熱膨脹係數高的氮化矽或碳化矽,但仍可維持低熱膨脹係數。此外,菫青石質燒結體因為含有比菫青石楊氏模數高的氮化矽或碳化矽,其剛性比單獨菫青石高。再者,此菫青石質燒結體的開氣孔率為0.5%以下,幾乎不含有氣孔,平均粒徑為1μm以下,研磨加工面(研磨面)的平坦性變高。 The flatilite sintered system of this embodiment is mainly composed of flatilite and contains silicon nitride or silicon carbide. The main component refers to the component with the largest volume in the sintered body. It is preferable that the sintered body made of flatilite has a thermal expansion coefficient of less than 2.4 ppm/°C at 40 to 400°C, an open porosity of 0.5% or less, and an average crystal grain size of 1 μm or less. Although the sintered body of flatilite contains silicon nitride or silicon carbide, which has a higher coefficient of thermal expansion than that of flatilite, it can still maintain a low coefficient of thermal expansion. In addition, since the sintered body made of plastinite contains silicon nitride or silicon carbide with a higher Young's modulus than that of plastinite, its rigidity is higher than that of plastinite alone. In addition, the open porosity of the sintered balsamite is 0.5% or less, contains almost no pores, has an average particle size of 1 μm or less, and the flatness of the polished surface (polished surface) is improved.
本實施形態的菫青石質燒結體較佳每100μm×100μm面積中最大長度1μm以上的氣孔數為10個以下。若氣孔數在10個以下,則研磨加工面的平坦性變得更高。此氣孔數較佳為3個以下,更佳為0個。 It is preferable that the sintered body of vernilite of the present embodiment has 10 or less pores with a maximum length of 1 μm or more per an area of 100 μm×100 μm. If the number of pores is 10 or less, the flatness of the polished surface becomes higher. The number of pores is preferably 3 or less, more preferably 0.
本實施形態的菫青石質燒結體較佳楊氏模數為160GPa以上,4點彎曲強度為220MPa以上。因氮化矽或碳化 矽的楊氏模數或強度比菫青石高,利用調整對菫青石的添加比例,可使菫青石質燒結體的楊氏模數達160GPa以上,4點彎曲強度為220MPa以上。 It is preferable that the sintered body of vernilite of the present embodiment has a Young's modulus of 160 GPa or more and a 4-point bending strength of 220 MPa or more. Due to silicon nitride or carbonization The Young's modulus or strength of silicon is higher than that of flatidite. By adjusting the addition ratio of flatidite, the Young's modulus of the flatidite-based sintered body can reach 160GPa or more, and the 4-point bending strength can be 220MPa or more.
本實施形態的菫青石質燒結體較佳研磨面中心之平均粗度Ra為1.5nm以下。作為彈性波元件等使用的複合基板,已知為接合機能性基板與支持基板所製,因此使用研磨面Ra為1.5nm以下之菫青石質燒結體作為支持基板,可使支持基板與機能性基板的接合性良好。例如,接合界面中實際接合的面積比例(接合面積比例)為80%以上(較佳為90%以上)。研磨面的中心平均粗度Ra為1.1nm以下,更佳為1.0nm以下,最佳為0.8nm以下。 It is preferable that the average roughness Ra of the center of the polished surface of the vernilite sintered body of this embodiment is 1.5 nm or less. As a composite substrate used for elastic wave devices, it is known to be made by joining a functional substrate and a support substrate. Therefore, a sintered sintered calalite with a polishing surface Ra of 1.5 nm or less is used as a support substrate to make the support substrate and the functional substrate The bonding is good. For example, the actual bonding area ratio (joining area ratio) in the bonding interface is 80% or more (preferably 90% or more). The center average roughness Ra of the polished surface is 1.1 nm or less, more preferably 1.0 nm or less, and most preferably 0.8 nm or less.
本實施形態的菫青石質燒結體較佳40~400℃熱膨脹係數為2.0ppm/℃以下。以菫青石質燒結體作為支持基板所形成的複合基板應用於彈性波元件,彈性波元件的溫度上升時,機能性基板具有比原本熱膨脹小的熱膨脹,可改善彈性波元件的頻率溫度依賴性。40~400℃熱膨脹係數較佳為1.8ppm/℃以下。 It is preferable that the sintered sintered body made of balsamite of this embodiment has a thermal expansion coefficient of 2.0 ppm/°C or less at 40 to 400°C. The composite substrate formed by using the sintered body of calalite as the supporting substrate is applied to the elastic wave device. When the temperature of the elastic wave device rises, the functional substrate has thermal expansion smaller than the original thermal expansion, which can improve the frequency-temperature dependence of the elastic wave device. The coefficient of thermal expansion at 40 to 400°C is preferably 1.8 ppm/°C or less.
本實施形態的菫青石質燒結體在含有氮化矽時,較佳菫青石相為60~90體積%,氮化矽相為10~40體積%,在含有碳化矽時,較佳菫青石相為70~90體積%,碳化矽相為10~30體積%。若為此組合比例,氣孔數或楊氏模數、研磨面的中心平均粗度Ra、40~400℃熱膨脹係數等特性良好。各相的體積%,以下述方式獲得。即,對於本實施形態菫青石質燒結體的研磨面,以SEM反射式電子顯微鏡進行影像觀察及組 成分析,以影像的菫青石比例獲得各相的面積比例,權宜上作為各相的體積比例(體積%)。 When the flatilite sintered body of this embodiment contains silicon nitride, the flatilite phase is preferably 60-90% by volume, and the silicon nitride phase is 10-40% by volume. When silicon carbide is contained, the flatilite phase is preferred. It is 70~90% by volume, and the silicon carbide phase is 10~30% by volume. With this combination ratio, the characteristics such as the number of pores or Young's modulus, the average roughness of the center of the polished surface Ra, and the coefficient of thermal expansion at 40 to 400°C are good. The volume% of each phase is obtained in the following manner. That is, for the polished surface of the sintered sintered body of calalite in this embodiment, image observation and assembly were performed with a SEM reflection electron microscope. Component analysis, the area ratio of each phase is obtained by the ratio of vernixite in the image, which is expediently used as the volume ratio (vol%) of each phase.
接著,對本發明菫青石質燒結體的製造方法之一實施形態進行說明。參照第1圖,菫青石質燒結體的製造包括(a)配製混合原料粉末的步驟,(b)製作菫青石質燒結體的步驟。 Next, an embodiment of the method for producing the sintered sintered body of vermilionite according to the present invention will be described. Referring to Fig. 1, the production of the sintered body includes (a) the steps of preparing a mixed raw material powder, and (b) the step of producing the sintered body of calalite.
步驟(a):混合原料粉末的製備 Step (a): Preparation of mixed raw material powder
菫青石原料較佳使用純度高,平均粒徑小的粉末。純度較佳為99.0%以上,更佳為99.5%以上,最佳為99.8%以上。純度的單位為質量%。此外,平均粒徑(D50)較佳為1μm以下,更佳為0.1~1μm。菫青石原料可為市售,也可使用高純度氧化鎂、氧化鋁、二氧化矽粉末製作。菫青石原料的製作方法可參照如專利文獻3所記載的方法。氮化矽原料或碳化矽原料較佳使用平均粒徑小的粉末。平均粒徑較佳為1μm以下,更佳為0.1~1μm。在配製菫青石原料與氮化矽原料的混合原料粉末時,例如,稱量60~90體積%菫青石原料與10~40體積%氮化矽原料,合計100體積%,以球磨機等混合機混合,必要時以噴霧乾燥機乾燥,以獲得混合原料粉末。此外,在配製菫青石原料與碳化矽原料的混合原料粉末時,例如,稱量70~90體積%菫青石原料與10~30體積%碳化矽原料,合計100體積%,以球磨機等混合機混合,必要時以噴霧乾燥機乾燥,以獲得混合原料粉末。
It is preferable to use a powder with high purity and a small average particle size as the raw material of flatilite. The purity is preferably 99.0% or more, more preferably 99.5% or more, and most preferably 99.8% or more. The unit of purity is mass %. In addition, the average particle diameter (D50) is preferably 1 μm or less, more preferably 0.1 to 1 μm. The raw material of flatilite can be commercially available, or it can be made of high-purity magnesia, alumina, and silica powder. For the production method of flatilite raw material, the method described in
步驟(b):菫青石質燒結體的製作 Step (b): Production of sintered body
由步驟(a)所獲得的混合原料粉末形成所定形狀的成形體。成形的方法並無特別限制,可使用一般的成形法。例如, 混合原料粉末直接以模具按壓成形。按壓成形時,可利用噴霧乾燥形成顆粒狀,成形性變得良好。此外,添加有機黏著劑,製作坏土,押出成形,製作泥漿以形成片狀。這些程序在燒成步驟前或燒成步驟中必須去除有機黏著劑。另外,也可使用CIP(冷間靜水加壓)高壓成形。 The mixed raw material powder obtained in step (a) forms a molded body of a predetermined shape. The molding method is not particularly limited, and general molding methods can be used. E.g, The mixed raw material powder is directly pressed into a mold. In press molding, spray drying can be used to form pellets, and the moldability becomes good. In addition, organic adhesives are added to make bad soil, extruded to form, and make mud to form flakes. These procedures must remove the organic adhesive before or during the firing step. In addition, CIP (cold hydrostatic pressure) high pressure forming can also be used.
接著,將所獲得的成形體進行燒成,以製作菫青石質燒結體。此時,燒結粒子維持在微細狀態,燒結中氣孔的排出可提升菫青石質燒結體表面的平坦性。此方法對熱壓法非常有效。比起常溫燒結,使用此熱壓法在低溫下可增進微細粒子狀態的緻密化,抑制常溫燒結中常見的粗大氣孔。熱壓時的燒成溫度較佳為1350~1450℃,更佳為1375~1425℃。此外,熱壓時的壓力較佳為20~300kgf/cm2。特別是低的壓力可使熱壓治具小型化及延長壽命。燒成溫度(最高溫度)的保持時間可考量成形體的形狀或大小、加熱爐的特性等,選擇適合、適當的時間。具體上較佳的保持時間,如1~12小時,更佳為2~8小時。燒成環境並無特別限制,熱壓時的環境可為一般氮氣、氬氣等惰性氣體環境。升溫速度或降溫速度可考量成形體的形狀或大小、加熱爐的特性等,進行適合、適當的設定,例如,可設定為50~300℃/hr的範圍。 Next, the obtained molded body is fired to produce a flatilite sintered body. At this time, the sintered particles are maintained in a fine state, and the discharge of pores during sintering can improve the flatness of the surface of the sintered sintered body. This method is very effective for hot pressing. Compared with normal temperature sintering, the use of this hot pressing method can improve the densification of the fine particle state at low temperatures, and suppress the common large air pores in normal temperature sintering. The firing temperature during hot pressing is preferably 1350 to 1450°C, more preferably 1375 to 1425°C. In addition, the pressure during hot pressing is preferably 20 to 300 kgf/cm 2 . In particular, the low pressure can miniaturize the hot press fixture and prolong its life. The holding time of the firing temperature (maximum temperature) can be selected for an appropriate and appropriate time in consideration of the shape or size of the molded body, the characteristics of the heating furnace, and the like. Specifically, the preferred holding time is, for example, 1 to 12 hours, and more preferably 2 to 8 hours. The firing environment is not particularly limited, and the environment during the hot pressing can be an inert gas environment such as general nitrogen and argon. The heating rate or cooling rate can be appropriately and appropriately set in consideration of the shape or size of the molded body, the characteristics of the heating furnace, and the like. For example, it can be set in the range of 50 to 300°C/hr.
接著,對本發明複合基板之一實施形態進行說明。本實施形態的複合基板為機能性基板與上述菫青石質燒結體所製之支持基板接合而成。此複合基板可增加兩基板的接合面積,以具有良好的接合特性。機能性基板並無特別限制,例如,擇自鉭酸鋰、鈮酸鋰、氮化鎵、二氧化矽等。接合方法較
佳為直接接合。直接接合時,在分別研磨機能性基板和支持基板的接合面後,進行活性化,將兩接合面以相互面對的狀態按壓兩基板。接合面的活性化,例如以惰性氣體(氬等)離子束、電漿或中性原子束等照射接合面。機能性基板與支持基板的厚度比(機能性基板厚度/支持基板厚度)較佳為0.1以下。第2圖顯示複合基板之一例子。複合基板10係將作為機能性基板的壓電基板12與支持基板14以直接接合的方式接合而成。
Next, an embodiment of the composite substrate of the present invention will be described. The composite substrate of the present embodiment is formed by joining a functional substrate and a support substrate made of the above-mentioned flatilite sintered body. The composite substrate can increase the bonding area of the two substrates to have good bonding characteristics. The functional substrate is not particularly limited. For example, it is selected from lithium tantalate, lithium niobate, gallium nitride, silicon dioxide, and the like. Bonding method is more
Best for direct bonding. In the case of direct bonding, the bonding surfaces of the functional substrate and the support substrate are separately polished and then activated, and the two bonding surfaces are pressed against the two substrates in a state where they face each other. To activate the bonding surface, for example, the bonding surface is irradiated with an inert gas (argon, etc.) ion beam, plasma, or neutral atom beam. The thickness ratio of the functional substrate and the support substrate (functional substrate thickness/support substrate thickness) is preferably 0.1 or less. Figure 2 shows an example of a composite substrate. The
本實施形態的複合基板可作為電子元件使用。此電子元件在彈性波元件(彈性表面波元件或藍姆波、薄膜共振器(FBAR))上,可擇自LED元件、光導波元件、開關元件等。彈性波元件在利用上述複合基板時,因作為支持基板之菫青石質燒結體的熱膨脹系數為非常小的未滿2.4ppm/℃(40~400℃),可大幅地改善頻率溫度依賴性。第3圖顯示使用複合基板10製作的電子元件30之一例子。電子元件30為One Port SAW共振器,即彈性表面波元件。首先,使用一般的光蝕刻在複合基板10的壓電基板12上形成複數個電子元件30的圖樣,之後切割出一個一個電子元件30。電子元件30利用光蝕刻技術在壓電基板12的表面上形成IDT(Interdigital Transducer)電極32、34與反射電極36。
The composite substrate of this embodiment can be used as an electronic component. This electronic component can be selected from LED components, optical waveguide components, switching components, etc. on elastic wave components (surface acoustic wave components or Lamb waves, thin film resonators (FBAR)). When the elastic wave element uses the above-mentioned composite substrate, since the thermal expansion coefficient of the sintered sintered body of calalite as the supporting substrate is very small and less than 2.4 ppm/°C (40 to 400°C), the frequency temperature dependence can be greatly improved. FIG. 3 shows an example of an
上述實施例不可用於限定本發明,本發明的技術範圍對本發明進行說明,也不限於本發明。 The above-mentioned embodiments cannot be used to limit the present invention, and the technical scope of the present invention describes the present invention, and is not limited to the present invention.
【實施例】 [Examples]
1.混合原料粉末的製作 1. Production of mixed raw material powder
首先,使用市售平均粒徑1μm以下,純度99.9%以上的高 純度氧化鎂、氧化鋁、二氧化矽粉末製作菫青石原料。換言之,以形成菫青石組成物為目的將各粉末進行秤重,混合,於1400℃大氣環境下加熱5小時,以獲得菫青石粗顆粒物。對所獲得的菫青石粗顆粒物,以氧化鋁作為圓石( 3mm),在使用純水之球磨機中進行70小時粉碎,以製作平均粒徑0.5~0.6μm的菫青石粉碎物。將所獲得的泥漿在大氣下,以110℃進行乾燥,藉由篩選乾燥物獲得菫青石粉末。依表一中實驗例1~9的原料粉末組成比例,秤量菫青石原料與氮化矽原料或碳化矽原料,藉由使用 5mm氧化鋁圓石的球磨機混合,利用噴霧乾燥製作混合原料粉末。此外,氮化矽原料可為市售平均粒徑0.8μm,純度97%以上的粉末,碳化矽原料可為市售平均粒徑0.5μm,純度97%以上的粉末。 First, use commercially available high-purity magnesia, alumina, and silica powders with an average particle size of 1 μm or less and a purity of 99.9% or more to make the raw material of flamite. In other words, the powders are weighed and mixed for the purpose of forming the flatilite composition, and heated at 1400° C. for 5 hours in an atmospheric environment to obtain coarse flatilite particles. For the obtained coarse particles of glazeite, alumina was used as the cobblestone ( 3mm), pulverized in a ball mill using pure water for 70 hours to produce pulverized glazeite with an average particle diameter of 0.5 to 0.6 μm. The obtained slurry was dried at 110° C. under the atmosphere, and the dried product was sieved to obtain flaxite powder. According to the composition ratio of the raw material powder in Experimental Examples 1-9 in Table 1, weigh the calalite raw material and the silicon nitride raw material or silicon carbide raw material by using The 5mm alumina pebbles are mixed with a ball mill and spray-dried to produce mixed raw material powder. In addition, the silicon nitride raw material can be a commercially available powder with an average particle size of 0.8 μm and a purity of more than 97%, and the silicon carbide raw material can be a commercially available powder with an average particle size of 0.5 μm and a purity of more than 97%.
2.菫青石質燒結體的製作 2. Production of sintered body of plastinite
實驗例1~9的混合原料粉末以50kgf/cm2單軸模具進行壓力成形,以獲得 100mm厚度25mm的成形體。將各成形體置於石墨製的模具中,使用熱壓爐,在200kgf/cm2壓力下,以1375~1425℃燒成溫度(最高溫度)進行5小時燒成,以製作菫青石質燒結體。各實驗例的燒成溫度如表一所示。燒成環境為氬氣環境,升溫速度為100℃/hr,降溫速度為200℃/hr,降溫時從1200℃以下退火。此外,實驗例10僅使用菫青石粉末,以相同條件製作成形體,使用熱壓爐,在壓力200kgf/cm2下,以1425℃燒成溫度(最高溫度),進行5小時燒成,以製作單獨菫青石的燒結體。 The mixed raw material powders of experimental examples 1 to 9 were pressure-formed with a 50kgf/cm 2 uniaxial mold to obtain A molded body with a thickness of 100mm and a thickness of 25mm. Place each molded body in a graphite mold and use a hot-press furnace to fire at a sintering temperature (maximum temperature) of 1375 to 1425°C for 5 hours under a pressure of 200 kgf/cm 2 to produce a sintered body of vermilionite . The firing temperature of each experimental example is shown in Table 1. The firing environment is an argon atmosphere, the temperature rise rate is 100°C/hr, the temperature drop rate is 200°C/hr, and the annealing is carried out from 1200°C or lower when the temperature is lowered. In addition, experimental example 10 uses only vermilionite powder to produce a molded body under the same conditions, using a hot press furnace, at a pressure of 200 kgf/cm 2 and a sintering temperature of 1425°C (maximum temperature) for 5 hours to produce A sintered body of glazeite alone.
3.特性評估 3. Characteristic evaluation
由實驗例1~10的菫青石質燒結體,切片出試驗片(4×3×40mm的抗折棒),以進行評估試驗。此外,燒結體的研磨面可藉由研磨4×3×10mm試驗片的一面,加工形成鏡面狀。依序使用3μm鑽石顆粒、0.5μm鑽石顆粒進行研磨,最後以0.1μm以下的鑽石顆粒進行最後的研磨修飾。特性的評估如下所述。 Test pieces (4×3×40 mm anti-bending rods) were sliced from the vermilion sintered bodies of Experimental Examples 1 to 10 for evaluation tests. In addition, the polished surface of the sintered body can be processed into a mirror surface by polishing one surface of a 4×3×10 mm test piece. Use 3μm diamond particles, 0.5μm diamond particles for grinding in sequence, and finally with diamond particles below 0.1μm for final grinding and modification. The evaluation of the characteristics is as follows.
(1)結晶相 (1) Crystalline phase
粉碎燒結體,利用X光繞射儀進行結晶相的測定。測定條件為CuKα、50kV、300mA、2θ=5-70°。使用旋轉對陰極型X光繞射儀(理學電極製RINT)。 The sintered body is pulverized, and the crystal phase is measured with an X-ray diffraction apparatus. The measurement conditions are CuKα, 50kV, 300mA, 2θ=5-70°. A rotating counter-cathode X-ray diffractometer (RINT manufactured by Rigaku Electrode) was used.
(2)燒結體的組成 (2) Composition of sintered body
對上述完成的燒結體研磨面,以SEM進行反射電子顯像觀察及組成分析,由影像對比率求得菫青石相與其它結晶相的面積比率,以此作為燒結體的體積比率。第4圖顯示研磨面 SEM影像之一例子。第4圖為實驗例3菫青石質燒結體研磨面的SEM影像,(a)為原始數據,(b)為二值化處理後的數據。第4(a)圖中,黑色部分為菫青石相,白色部分為氮化矽相。 The polished surface of the sintered body was observed by reflection electron imaging and composition analysis by SEM, and the area ratio of the vermilion phase to other crystalline phases was obtained from the image contrast ratio, which was used as the volume ratio of the sintered body. Figure 4 shows the ground surface An example of SEM image. Figure 4 is an SEM image of the polished surface of the sintered body of vermilionite in Experimental Example 3. (a) is the original data, and (b) is the data after the binarization process. In Figure 4(a), the black part is the calalite phase, and the white part is the silicon nitride phase.
(3)容積密度、開氣孔率 (3) Bulk density, open porosity
使用抗折棒,藉由使用純水的阿基米德法,測定容積密度、開氣孔率。 Measure the bulk density and open porosity by the Archimedes method using pure water using an anti-folding rod.
(4)相對密度 (4) Relative density
由燒結體的組成及各成分密度計算出燒結體的計算密度,以上述所測定的容積密度與計算密度的比例作為相對密度。在本發明中,菫青石的密度為2.505g/cm3,氮化矽密度為3.20g/cm3,碳化矽密度為3.21g/cm3。本發明所使用之氮化矽、碳化矽的密度不考慮原料中雜質氧等的影響。 The calculated density of the sintered body is calculated from the composition of the sintered body and the density of each component, and the ratio of the measured bulk density to the calculated density is taken as the relative density. In the present invention, pansy bluestone density 2.505g / cm 3, a silicon nitride density of 3.20g / cm 3, silicon carbide density of 3.21g / cm 3. The density of silicon nitride and silicon carbide used in the present invention does not consider the influence of impurity oxygen in the raw material.
(5)彎曲強度 (5) Bending strength
依據JIS R1601準則,測定4點彎曲強度。試驗片的形狀為3×4×40mm抗折棒或其一半長度的抗折棒。 According to JIS R1601, the 4-point bending strength is measured. The shape of the test piece is a 3×4×40 mm anti-folding rod or a half-length anti-folding rod.
(6)楊氏模數 (6) Young's modulus
依據JIS R1602準則,以靜態扭曲法進行測定。試驗片的形狀為3×4×40mm抗折棒。 According to the JIS R1602 standard, it is measured by the static torsion method. The shape of the test piece is a 3×4×40 mm anti-folding rod.
(7)熱膨脹係數(40~400℃) (7) Thermal expansion coefficient (40~400℃)
依據JIS R1618準則,以壓棒示差法進行測定。試驗片的形狀為3×4×20mm抗折棒。 According to the JIS R1618 standard, the measurement is carried out by the pressure bar differential method. The shape of the test piece is a 3×4×20 mm anti-folding rod.
(8)氣孔數 (8) Number of stomata
以SEM觀察上述完成的燒結體研磨面,計數每100μm×100μm中所存在最大長度為1μm以上的氣孔數量。 The polished surface of the completed sintered body was observed by SEM, and the number of pores with a maximum length of 1 μm or more per 100 μm×100 μm was counted.
(9)表面平坦性(Ra) (9) Surface flatness (Ra)
對於上述完成的燒結體研磨面,使用AFM測定中心性平均粗度Ra。測定範圍為10μm×10μm。 With respect to the polished surface of the sintered body completed as described above, the centrality average roughness Ra was measured using AFM. The measurement range is 10μm×10μm.
(10)燒結粒子的平均粒徑 (10) Average particle size of sintered particles
對於上述完成的燒結體研磨面,在1200~1400℃下進行2小時的熱蝕刻,利用SEM測定200個以上燒結粒子的大小,使用線性分析計算平均粒徑。線性分析係數為1.5,以SEM所測定的長度乘以1.5作為平均粒徑。 For the polished surface of the sintered body completed above, thermal etching was performed at 1200 to 1400°C for 2 hours, the size of 200 or more sintered particles was measured by SEM, and the average particle size was calculated by linear analysis. The linear analysis coefficient is 1.5, and the length measured by SEM is multiplied by 1.5 as the average particle size.
(11)接合性 (11) Joinability
由實驗例1~10的燒結體切割出直徑100mm、厚度600μm的圓板。依上述法方將此圓板研磨加工後,清洗表面以去除顆粒或汙染物質等。接著,以此圓板作為支持基板,將支持基板與機能性基板直接接合以獲得複合基板。換言之,首先分別將支持基板與機能性基板的接合面以氬離子束活化,接著將兩接合面相互面對,以10tonf按壓,以獲得接合的複合基板。機能性基板可使用鉭酸鋰(LT)基板和鈮酸鋰(LN)基板。接合性的評估透過紅外線影像進行判斷,接合面積達90%為「最佳」,80%以上90%以下為「佳」,80%以下為「不佳」。 Discs with a diameter of 100 mm and a thickness of 600 μm were cut from the sintered bodies of Experimental Examples 1-10. After grinding and processing the disc according to the above method, the surface is cleaned to remove particles or pollutants. Next, the disc is used as a supporting substrate, and the supporting substrate and the functional substrate are directly bonded to obtain a composite substrate. In other words, firstly, the bonding surfaces of the supporting substrate and the functional substrate are activated with an argon ion beam, and then the two bonding surfaces are faced to each other and pressed at 10 tonf to obtain a bonded composite substrate. As a functional substrate, a lithium tantalate (LT) substrate and a lithium niobate (LN) substrate can be used. The bonding property is evaluated through infrared images. A bonding area of 90% is considered "best", 80% or more and 90% or less is "good", and 80% or less is "not good".
4.評估結果 4. Evaluation results
與實驗例10的單獨菫青石燒結體相比,含有氮化矽或碳化矽之實驗例1~9的菫青石質燒結體,彎曲強度及楊氏模數增加。楊氏模數提升至160GPa以上,4點彎曲強度為220MPa以上。此外,實驗例1~4、6~8的菫青石質燒結體,其40~400℃的熱膨脹係數未滿2.4ppm/℃(添加氮化矽之實驗例1~4為1.4~1.8ppm/℃, 添加碳化矽之實驗例6~8為1.8~2.3ppm/℃),雖然與實驗例10的單獨菫青石燒結體相比稍微增加,但仍維持低的熱膨脹係數。再者,實驗例1~4、6~8的菫青石質燒結體,其開氣孔率未滿0.1%,平均結晶粒徑為1μm以下,研磨面的中心平均粗度Ra變為1.1nm以下。因此,由實驗例1~3、6、7菫青石質燒結體切割出的圓板與機能性基板直接接合的接合性為兩者接合面積90%以上的「最佳」,由實驗例4、8菫青石質燒結體切割出的圓板與機能性基板直接接合時的接合性為接合面積80%以上90%以下的「佳」。此外,研磨面的中心平均粗度Ra變為此低值時,有助於使氣孔數減少至3個以下。此外,實驗例1~9平均粒徑變為1μm以下的原因之一,為沒有使用稀土類氧化物助燒結劑進行燒結。 Compared with the sintered body of pure vermilionite of Experimental Example 10, the sintered body of vermilionite of Experimental Examples 1 to 9 containing silicon nitride or silicon carbide has increased flexural strength and Young's modulus. The Young's modulus is increased to more than 160 GPa, and the 4-point bending strength is more than 220 MPa. In addition, the sintered bodies of vermilionite of Experimental Examples 1 to 4 and 6 to 8 have a thermal expansion coefficient of less than 2.4 ppm/°C at 40 to 400°C (Experimental Examples 1 to 4 with silicon nitride added are 1.4 to 1.8 ppm/°C) , The experimental examples 6 to 8 where silicon carbide was added were 1.8 to 2.3 ppm/°C). Although it was slightly increased compared with the sintered vermilionite alone of experimental example 10, the coefficient of thermal expansion was still low. In addition, the open porosity of the vermilionite sintered bodies of Experimental Examples 1 to 4 and 6 to 8 was less than 0.1%, the average crystal grain size was 1 μm or less, and the center average roughness Ra of the polished surface was 1.1 nm or less. Therefore, the bonding performance between the discs cut out of the sintered bodies of vermilionite and the functional substrate in the experimental examples 1 to 3, 6, and 7 is the "best" which is 90% or more of the bonding area of the two. According to the experimental examples 4, 8 When the disc cut out of the sintered plastinite body is directly bonded to the functional substrate, the bonding performance is "good", which is 80% or more and 90% or less of the bonding area. In addition, when the average center roughness Ra of the polished surface becomes this low value, it contributes to reducing the number of pores to 3 or less. In addition, one of the reasons why the average particle size of Experimental Examples 1 to 9 became 1 μm or less was that the rare earth oxide sintering aid was not used for sintering.
另外,實驗例1~4、6~8相當於本發明的實施例,實驗例5、9、10相當於比較例。此實驗例不可用於限定本發明。 In addition, Experimental Examples 1 to 4 and 6 to 8 correspond to Examples of the present invention, and Experimental Examples 5, 9, and 10 correspond to Comparative Examples. This experimental example cannot be used to limit the present invention.
本發明基於主張於2016年3月23日申請之日本專利申請號2016-058969號以及2017年2月24日申請之日本專利申請號2017-033437號優先權,其內容被引用至本發明說明書中。 The present invention is based on claiming the priority of Japanese Patent Application No. 2016-058969 filed on March 23, 2016 and Japanese Patent Application No. 2017-033437 filed on February 24, 2017, the contents of which are cited in the specification of the present invention .
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