JPS63270303A - Regeneration of phosphoric acid - Google Patents
Regeneration of phosphoric acidInfo
- Publication number
- JPS63270303A JPS63270303A JP10279087A JP10279087A JPS63270303A JP S63270303 A JPS63270303 A JP S63270303A JP 10279087 A JP10279087 A JP 10279087A JP 10279087 A JP10279087 A JP 10279087A JP S63270303 A JPS63270303 A JP S63270303A
- Authority
- JP
- Japan
- Prior art keywords
- phosphoric acid
- concentration
- heating
- precipitate
- dissolved
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 70
- 230000008929 regeneration Effects 0.000 title 1
- 238000011069 regeneration method Methods 0.000 title 1
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 239000002244 precipitate Substances 0.000 claims description 19
- 238000007788 roughening Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 230000001172 regenerating effect Effects 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 4
- -1 Al metal Chemical class 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052863 mullite Inorganic materials 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 3
- 229910017083 AlN Inorganic materials 0.000 abstract 1
- 235000011007 phosphoric acid Nutrition 0.000 description 58
- 239000000203 mixture Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- DHAHRLDIUIPTCJ-UHFFFAOYSA-K aluminium metaphosphate Chemical compound [Al+3].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O DHAHRLDIUIPTCJ-UHFFFAOYSA-K 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 150000003016 phosphoric acids Chemical class 0.000 description 3
- 229910018626 Al(OH) Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- ing And Chemical Polishing (AREA)
Abstract
Description
【発明の詳細な説明】
〔技術分野〕
本発明は、セラミック基板表面の粗面化処理に使用され
るリン酸の再生方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method for regenerating phosphoric acid used for roughening the surface of a ceramic substrate.
アルミニウムを含むセラミック配線回路板は、加熱した
リン酸により、セラミック基板表面を粒面化処理した後
、メタライズ処理を行なうことにより製造される。A ceramic printed circuit board containing aluminum is manufactured by subjecting the surface of a ceramic substrate to graining treatment using heated phosphoric acid, and then performing metallization treatment.
前記セラミック基板表面を加熱したリン酸により粗面化
処理した後メタライズし、セラミック配線回路板を製造
する技術は特開昭６０−４６９７６号公報、特開昭６１
−１５９７９２号公報等に見られる。A technique for manufacturing a ceramic wiring circuit board by roughening the surface of the ceramic substrate with heated phosphoric acid and then metalizing it is disclosed in Japanese Patent Laid-Open Nos. 60-46976 and 61.
-159792, etc.
たとえば、７５〜９０ｗｔ％のリン酸（Ｈ３Ｐ０４）を
、２５０〜３６０℃に加熱し、９２〜９９％のアルミナ
ＣＡ１ｚ ｏ、）基板を３〜１０分浸漬することにより
、基板表面を粗面化している。つぎに、メタライズ処理
として化学銅メッキ処理を行ない、基板表面に導体層を
形成させ、セラミック配線回路板を製造する。For example, by heating 75 to 90 wt% phosphoric acid (H3P04) to 250 to 360 °C and immersing a 92 to 99% alumina CA1ZO,) substrate for 3 to 10 minutes, the substrate surface can be roughened. There is. Next, a chemical copper plating process is performed as a metallization process to form a conductor layer on the surface of the substrate, thereby producing a ceramic printed circuit board.
ところが、Ａｌ、Ｏ，基板表面を粗面化する場合、加熱
リン酸は基板表面の粒界およびブレーンを攻撃し、Ａｌ
、Ｏ，ブレーンを脱落させ、溶解する。したがって、基
板の粗面化処理を繰りかえずごとに、リン酸中のアルミ
ニウム（Ａ ｌ ） 濃度は高くなり、粗面化処理能力
が低下するという問題が生じた。However, when roughening the surface of an Al, O, or substrate, heated phosphoric acid attacks the grain boundaries and branes on the substrate surface,
, O, the brane falls off and dissolves. Therefore, each time the surface roughening treatment of the substrate is repeated, the concentration of aluminum (A l ) in the phosphoric acid increases, resulting in a problem that the surface roughening treatment ability decreases.
また、粗面化処理には、多量のリン酸を使用）゛るため
、生じる廃リン酸をどう処理するかが問題となった。こ
のことから、粗面化処理能力をほとんど低下させること
なくリン酸を再生し、リサイクル使用できるにようにす
る技術が要望されていた。Furthermore, since a large amount of phosphoric acid is used in the surface roughening treatment, there was a problem of how to dispose of the waste phosphoric acid produced. For this reason, there has been a demand for a technology that allows phosphoric acid to be regenerated and recycled without substantially reducing the surface roughening treatment capacity.
本発明の目的は、アルミニウムを含有するセラミック基
板表面の粗面化処理に使用したリン酸を、粗面化処理能
力をほとんど低下させることなく、再生する方法を提供
することを目的とする。An object of the present invention is to provide a method for regenerating phosphoric acid used for roughening the surface of a ceramic substrate containing aluminum, without substantially reducing the roughening treatment ability.
本発明は、アルミニウムを含イｊするセラミック基板表
面の粗面化処理に使用したリン酸にＡ７！含有化合物を
添加し、ＡｌｐＱ度を高めた後、加熱することにより沈
殿物を析出させて除去することを、その要旨とするもの
である。The present invention uses A7! phosphoric acid for roughening the surface of a ceramic substrate containing aluminum. The gist of the method is to add a compound to increase the AlpQ degree, and then heat to precipitate and remove the precipitate.
本発明は、Ａｌ２Ｏ３、ムライト、ＡＩＮ等のＡｆｆが
主成分となるセラミック基板を、リン酸すなわちオルト
リン酸、ピロリン酸、メタリン酸等の１種またはこれら
の混合物を加熱したものにより、セラミック基板表面を
粗面化処理した時に生じる、Ａ１を溶存するリン酸に対
し適用される。In the present invention, the surface of a ceramic substrate mainly composed of Aff such as Al2O3, mullite, and AIN is heated with phosphoric acid, that is, one of orthophosphoric acid, pyrophosphoric acid, metaphosphoric acid, etc., or a mixture thereof. It is applied to phosphoric acid in which A1 is dissolved, which is generated during surface roughening treatment.
リン酸中に溶存するＡ Ｉ−？帰度は、下記の第１式で
定義し、好ましくはへｌ濃度０．１％以上のものに対し
適用される。A I-? dissolved in phosphoric acid? The degree of return is defined by the first equation below, and is preferably applied to a helium concentration of 0.1% or more.
×１００・・・・・・第１式
本発明は、リン酸中に溶存するＡｆが、加熱することに
より、リン酸に不）容のメタリン酸アルミニウム（Ａ
ｌ （Ｐ Ｏｓ）：＋ ）に変化することを利用したも
のであるが、加熱の際にＡＪ含有化合物をリン酸に添加
し、好ましくは溶解させてリン酸中の／ｌ濃度を高める
ことにより、Ａ Ａ！ （Ｐ Ｏ：ｌ）：１の結晶核
を多数生成させ、沈殿物の生成を促進するものである。×100... Formula 1 In the present invention, by heating Af dissolved in phosphoric acid, aluminum metaphosphate (A
This method takes advantage of the fact that the AJ-containing compound changes to 1 (POs): + ), but by adding an AJ-containing compound to phosphoric acid during heating and preferably dissolving it to increase the /1 concentration in phosphoric acid. , A A! It generates a large number of crystal nuclei of (P O:l):1 and promotes the formation of precipitates.
以下、詳しく説明する。This will be explained in detail below.
まず、粗面化に使用したリン酸中のＡ ｌ 濃度を高め
る。First, the Al concentration in the phosphoric acid used for surface roughening is increased.
リン酸中に、ＡＪ含有化合物を添加しＡ ｐ ｐＱ度を
、好ましくは０．６〜１．０％に高める。Ａ１含有化合
物としては、特に限定はないが、Ａｌ。An AJ-containing compound is added to phosphoric acid to increase the A p pQ degree, preferably from 0.6 to 1.0%. The A1-containing compound is not particularly limited, but includes Al.
Ｏｗｌ 、Ａ ｌ （ＯＨ） ３等のＡＩ！以外の金属
イオンを含まないもの、Ａ ｅ （０２Ｐ ０４）ｚ
、Ａ ７！ＨｚＰ、０１゜等のリン酸塩、へ！金属粉
等が好ましい。また、ＡＮ含有化合物を添加した場合、
大抵は溶解するが、溶解しにくい場合は、リン酸を加熱
する時に加えてもかまわない。このようにしてリン酸中
のＡｌ ｅｉ度を高める場合、０．６％未満では、加熱
により形成される結晶核が少なくなり、加熱に長時間を
要し、また、１％をこえると、リン酸の消費量が増し再
生されるリン酸量が減少し、好ましくない。Owl, A l (OH) 3rd class AI! Those that do not contain metal ions other than A e (02P 04)z
, A 7! Phosphates such as HzP, 01°, etc., to! Metal powder and the like are preferred. In addition, when an AN-containing compound is added,
Most of the time it will dissolve, but if it is difficult to dissolve, you can add phosphoric acid when heating. When increasing the Al ei degree in phosphoric acid in this way, if it is less than 0.6%, fewer crystal nuclei will be formed by heating, and heating will take a long time; if it exceeds 1%, This is not preferable because the amount of acid consumed increases and the amount of phosphoric acid regenerated decreases.
つぎにリン酸の加熱を行なう。Next, phosphoric acid is heated.
ＡＩ濃度を高めたリン酸の加熱は、好ましくは２５０〜
５００℃で０．５〜３時間行なう。２５０°Ｃ未満では
沈殿物の析出に長時間を要し、また、５００℃を越える
と、リン酸自体の分解が進み、好ましくない。The heating of phosphoric acid with increased AI concentration is preferably performed at 250-250 ℃
It is carried out at 500°C for 0.5 to 3 hours. If the temperature is lower than 250°C, it will take a long time for the precipitation to occur, and if the temperature exceeds 500°C, the decomposition of the phosphoric acid itself will proceed, which is not preferable.
つぎに、好ましくは室温付近まで放冷し、加水分解を行
なわせる。つまり、加熱により脱水縮合し、高粘度とな
ったリン酸の粘度を下げ、沈殿物の除去を容易にする。Next, the mixture is preferably left to cool to around room temperature to carry out hydrolysis. That is, it reduces the viscosity of phosphoric acid, which has become highly viscous due to dehydration condensation due to heating, and facilitates the removal of precipitates.
さらに加水分解により縮合リン酸を分解して、つぎの粗
面化処理に使いやすいようにする。加える水量は、縮合
リン酸の好ましくは、２０〜４０ｗｔ％とし、さらに７
０〜９０℃で１〜２時間保持し、加水分解を行なわせる
最後に、口過、遠心分離等の分離法により生成した沈殿
物を除去する。この沈殿物をＸ線回折装置により分析を
行なったところ、主成分はメタリン酸アルミニウム（Ａ
ｘ （ＰＯ：＋）：＋ ）Ａタイプであることが確認
された。Furthermore, the condensed phosphoric acid is decomposed by hydrolysis, making it easier to use in the next surface roughening treatment. The amount of water added is preferably 20 to 40 wt% of the condensed phosphoric acid, and further 7
The mixture is maintained at 0 to 90° C. for 1 to 2 hours to perform hydrolysis. Finally, the precipitate produced is removed by a separation method such as filtration or centrifugation. When this precipitate was analyzed using an X-ray diffraction device, the main component was aluminum metaphosphate (A
x (PO:+):+) It was confirmed that it was A type.
この結果、リン酸中に溶存するＡ ｐ ｆＱ度は、０゜
１以下となる。また、この処理により再生したリン酸を
用いて、セラミック基板表面の粗面化処理を行なっても
、処理能力の低下はわずかであり、リン酸はリサイクル
使用できる。As a result, the degree of A p fQ dissolved in phosphoric acid becomes 0°1 or less. Further, even if the surface of the ceramic substrate is roughened using the phosphoric acid regenerated by this treatment, the processing capacity is only slightly reduced, and the phosphoric acid can be recycled.
つぎに、７５〜９０％リン酸を２５０〜３６０℃に加熱
し、９２〜９９％ＡｌｚＯ：＋基板を粗面化処理した際
に排出されたリン酸（Ａｊ！濃度Ｏ１２％）の場合につ
いて、具体的に説明する。Next, regarding the case of phosphoric acid (Aj! concentration O 12%) discharged when 75-90% phosphoric acid was heated to 250-360°C and a 92-99% AlzO:+ substrate was roughened, I will explain in detail.
まず、このリン酸にＡＩ含有化合物を溶解し八７！濃度
を高める。このリン酸に、Ａ ｐ ｃｉ度が、０．６〜
１．０％となるように、必要量の／ｌＩ！（Ｏｌｌ）、
を溶解した。First, an AI-containing compound is dissolved in this phosphoric acid. Increase concentration. This phosphoric acid has an Apci degree of 0.6 to
The required amount of /lI! to be 1.0%! (Oll),
was dissolved.
つぎに加熱を行なう。Next, heating is performed.
加熱は２５０〜５００℃で０．５〜３時間行なった。加
熱によりリン酸は白濁し、やがて沈殿物の析出がみられ
た。Heating was performed at 250-500°C for 0.5-3 hours. Upon heating, the phosphoric acid became cloudy, and soon a precipitate was observed.
第１図は、前記のＡ １ ？３度を高めたリン酸を３３
０℃に加熱した時、保持時間に対しリン酸中に溶存する
Ａ１濃度の変化を示したものである。曲線ａは、加熱時
にＡｌ （ＯＨ）ｚを加えてＡＩ濃度を０．８％に高め
た時に得られたものであり、曲線すは、Ａｆ（０１１）
ｚを加えずに加熱を行なった時のものである。FIG. 1 shows the above-mentioned A 1 ? Phosphoric acid with increased 3 degrees is 33
This figure shows the change in the concentration of A1 dissolved in phosphoric acid with respect to the holding time when heated to 0°C. Curve a was obtained when Al(OH)z was added during heating to increase the AI concentration to 0.8%;
This is when heating was performed without adding z.
第１図によれば、リン酸中のＡ １！ 濃度を、高める
ことにより、加熱時間は大幅に短縮された。この理由は
つぎのように考えられる。According to FIG. 1, A 1! in phosphoric acid! By increasing the concentration, the heating time was significantly shortened. The reason for this is thought to be as follows.
リン酸中に溶存するＡＩは、Ａ ｌ （Ｈｚ Ｐ ０
４）３の形で存在していると考えられるが、このＡｌ（
Ｈ２Ｐ ０ａ）３は加熱することにより脱水を行ない、
次式のように六β （ｐｏｉ）３の結晶核が生成される
。AI dissolved in phosphoric acid is A l (Hz P 0
4) It is thought that it exists in the form of 3, but this Al(
H2P 0a)3 is dehydrated by heating,
Six β (poi)3 crystal nuclei are generated as shown in the following equation.
ＡＡ （Ｈ２ＰＯ４） ３ ＝Ａｊ！Ｈｚ
Ｐ３ ０１０＋２ＨｚＯ
Ａ ｊ２ Ｈ□ Ｐ２Ｏ，。 →Ａ １２ （Ｐ ０
ｚ）３ →・Ｈ，０さらにこの核のまわりに、生成し
たＡｎ （ｒ’０３）、が成長していき、やがて沈殿物
となり析出する。AA (H2PO4) 3 = Aj! Hz
P3 010+2HzO A j2 H□ P2O,. →A 12 (P 0
z)3 →・H,0 Furthermore, the generated An (r'03) grows around this nucleus and eventually becomes a precipitate.
Ａｌ含有化合物を溶解し、Ａ １４度を高めることによ
り、Ａｅ？Ｑ度を高めないものに比べ、生成されるＡ
ｌ （Ｐ ０ｚ）３の結晶核の数は多くなり、Ａ ｌ
（Ｐ Ｏｎ）、の結晶の成長は促進され、短時間の加
熱により、リン酸中のＡｌｌを除去できるものと考えら
れる。By dissolving Al-containing compounds and increasing the A 14 degrees, Ae? Compared to those that do not increase the Q degree, the generated A
The number of crystal nuclei of l (P 0z)3 increases, and A l
It is thought that the growth of crystals of (P On) is promoted and that All in the phosphoric acid can be removed by short-term heating.
つぎに加水分解を行なう。Next, hydrolysis is performed.
加熱終了後、室温付近まで放冷し、リン酸の粘度を下げ
、沈殿物の除去を容易にするため、また、縮合したリン
酸を分解するため、加水分解を行なった。加水分解は、
得られたリン酸に対し、２０〜４０ｗｔ％の水を加え、
７０〜９０℃で１〜２時間行なわせた。水を添加するこ
とにより、リン酸は発熱を伴なってＨ，ＰＯ４に分解さ
れ、粘度は低下した。After heating, the mixture was allowed to cool to around room temperature, and hydrolysis was performed in order to lower the viscosity of the phosphoric acid and facilitate the removal of precipitates, and to decompose the condensed phosphoric acid. Hydrolysis is
Add 20 to 40 wt% of water to the obtained phosphoric acid,
It was carried out at 70-90°C for 1-2 hours. By adding water, phosphoric acid was decomposed into H and PO4 with heat generation, and the viscosity decreased.
最後に、沈殿物の除去を行なう。Finally, the precipitate is removed.
加水分解終了後、口過または遠心分離等の方法により、
生成した沈殿物を除去した。この沈殿物をＸ線回折装置
により分析したところ、主成分はメタリン酸アルミニウ
ｌ、（Ａ ｌ （Ｐ ０ｚ）ｉ ） Ａタイプであった
。また、Ｓ ｉ 、、Ｍ ｇ等のセラミック基板のフラ
ンクス成分も共沈して除去されることが、沈殿物の中に
リン酸塩の形で検出されることから明らかとなった。After completion of hydrolysis, by methods such as mouth filtration or centrifugation,
The generated precipitate was removed. When this precipitate was analyzed using an X-ray diffraction device, the main component was aluminum metaphosphate, (A l (P 0z)i ) A type. Furthermore, it has become clear that Franks components of the ceramic substrate, such as S i , M g , etc., are also coprecipitated and removed, as they are detected in the form of phosphates in the precipitate.
なお、沈殿物を除去して得られたリン酸中のＡ１ ’１
Ｆｊ＝度は、０．１％以下となり、このリン酸を再度用
いて、ＡＮｚＯｚ基板表面の粗面化処理を行なったとこ
ろ、処理能力の低下はわずかであり、リン酸のリサイク
ル使用は可能となった。In addition, A1 '1 in phosphoric acid obtained by removing the precipitate
Fj = 0.1% or less, and when this phosphoric acid was used again to roughen the surface of the ANzOz substrate, there was only a slight decrease in processing capacity, and it was possible to recycle the phosphoric acid. became.
（実施例１）
８５％Ｈ，ＰＯ４を用い、これを３３０”Ｃ４，：加熱
し、９６％Ａ７！、０３基板表面を粗化した。処理終了
後、リン酸中のＡｌ’（３度を測定したところ、０．３
％であった。(Example 1) Using 85% H, PO4, it was heated to 330" C4, to roughen the surface of the 96% A7!,03 substrate. After the treatment, Al' in phosphoric acid (3 degrees When measured, it was 0.3
%Met.
そこで、Ａ７！濃度が０．８％となるように、Ａ１ （
ＯＨ）：ｌを溶解させた後、３３０℃で１．５時間加熱
した。その後室温まで放冷した後、得られたリン酸に対
し３０ｗｔ％の水を加え、７０℃で２時間加水分解させ
た。So, A7! A1 (
After dissolving OH):l, it was heated at 330°C for 1.5 hours. After that, the mixture was allowed to cool to room temperature, and then 30 wt% of water was added to the obtained phosphoric acid, and the mixture was hydrolyzed at 70°C for 2 hours.
つぎに、遠心分離により沈殿物を除去した。Next, the precipitate was removed by centrifugation.
この沈殿物をＸ線回折装置により分析を行なったところ
、主成分はＡｊ２ （ＰＯ３）＋であった。When this precipitate was analyzed using an X-ray diffraction device, the main component was Aj2 (PO3)+.
その結果、リン酸中のＡｆｔａ度は０．１％以下となり
、再度粗面化処理に使用したところ、粗面化処理能力の
低下はわずかであり、リン酸をリサイクル使用できた。As a result, the degree of Afta in phosphoric acid was 0.1% or less, and when it was used again for surface roughening treatment, there was only a slight decrease in surface roughening treatment ability, and the phosphoric acid could be recycled.
（実施例２）
実施例１において、Ａｌ（ＯＨ）ｓの代わりにＡＪｔＯ
，を必要量加えた。この時、Ａｌｔｏｓの溶解は３００
℃にリン酸を加熱して行ない。ざらに３３０℃で１．５
時間保持した。(Example 2) In Example 1, AJtO was used instead of Al(OH)s.
, was added in the required amount. At this time, the melting rate of Altos is 300
This is done by heating phosphoric acid to ℃. Roughly 1.5 at 330℃
Holds time.
その結果、実施例１と同様の結果が得られた。As a result, the same results as in Example 1 were obtained.
（実施例３）
実施例１において、加熱条件を３６０℃、１時間とした
ところ、実施例１と同様の結果が得られた。(Example 3) In Example 1, when the heating conditions were set to 360° C. for 1 hour, the same results as in Example 1 were obtained.
（実施例４）
７５％Ｈ３１’０４を３６０℃に加熱し、９９％Ａ７！
ｚ○３基板表面を粗化した。この時、Ａ７！濃度を測定
したところ、０．２％であった。(Example 4) 75% H31'04 was heated to 360°C and 99% A7!
The surface of the z○3 substrate was roughened. At this time, A7! When the concentration was measured, it was 0.2%.
そこで、Ａｌ濃度が１％となるようにＡｌ（０！■）、
を溶解させた後、３３０℃で１．５時間加熱した。実施
例１と同様に加水分解及び沈殿物の除去を行なったとこ
ろ同様の結果が得られた。Therefore, Al(0!■), so that the Al concentration is 1%,
After dissolving, the mixture was heated at 330°C for 1.5 hours. Hydrolysis and removal of the precipitate were carried out in the same manner as in Example 1, and the same results were obtained.
（実施例５）
実施例４において、Ａｌ （ＯＨ）３の代わりにＡ ｌ
ｚ Ｏ３を必要量溶解させた。この時、ＡＩ。(Example 5) In Example 4, Al(OH)3 was replaced by Al
z O3 was dissolved in the required amount. At this time, AI.
０３の溶解は３００℃で行ない、さらに３６０℃で１時
間保持した。その結果、実施例１と同様の結果が得られ
た。03 was dissolved at 300°C and further held at 360°C for 1 hour. As a result, the same results as in Example 1 were obtained.
〔発明の効果〕
本発明は、セラミック基板表面の粗面化処理に使用した
リン酸に／ｌ含有化合物を溶解し、Ａ１濃度を高めた後
加熱を行ない、沈殿物を析出させて除去することにより
、リン酸の粗面化処理能力をほとんど低下させず、再生
することができ、リン酸の有効利用をはかることができ
る効果がある。[Effects of the Invention] The present invention involves dissolving a /l-containing compound in phosphoric acid used for roughening the surface of a ceramic substrate, increasing the A1 concentration, heating it, and depositing and removing a precipitate. This has the effect that phosphoric acid can be regenerated without substantially reducing its surface roughening treatment ability, and that phosphoric acid can be used effectively.
第１図は、リン酸中に溶存するＡｌ濃度を加熱時間に対
してプロットしたグラフである。FIG. 1 is a graph in which the concentration of Al dissolved in phosphoric acid is plotted against heating time.
Claims (1)
処理に使用したリン酸に、アルミニウム含有化合物を添
加し、アルミニウム濃度を高めて加熱することにより沈
殿物を析出させ、この沈殿物を除去することを特徴とす
るリン酸の再生方法。(1) Adding an aluminum-containing compound to phosphoric acid used for roughening the surface of a ceramic substrate containing aluminum, increasing the aluminum concentration and heating to precipitate a precipitate, and then removing this precipitate. A method for regenerating phosphoric acid, characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10279087A JPS63270303A (en) | 1987-04-24 | 1987-04-24 | Regeneration of phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10279087A JPS63270303A (en) | 1987-04-24 | 1987-04-24 | Regeneration of phosphoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63270303A true JPS63270303A (en) | 1988-11-08 |
Family
ID=14336912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10279087A Pending JPS63270303A (en) | 1987-04-24 | 1987-04-24 | Regeneration of phosphoric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63270303A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008189537A (en) * | 2007-02-08 | 2008-08-21 | Nippon Refine Kk | Method and apparatus for obtaining refined phosphoric acid from aqueous phosphoric acid solution containing a plurality of metal ions |
-
1987
- 1987-04-24 JP JP10279087A patent/JPS63270303A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008189537A (en) * | 2007-02-08 | 2008-08-21 | Nippon Refine Kk | Method and apparatus for obtaining refined phosphoric acid from aqueous phosphoric acid solution containing a plurality of metal ions |
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